JP2017186220A - 遷移金属酸化物含有二酸化セリウム粒子 - Google Patents
遷移金属酸化物含有二酸化セリウム粒子 Download PDFInfo
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- JP2017186220A JP2017186220A JP2016165006A JP2016165006A JP2017186220A JP 2017186220 A JP2017186220 A JP 2017186220A JP 2016165006 A JP2016165006 A JP 2016165006A JP 2016165006 A JP2016165006 A JP 2016165006A JP 2017186220 A JP2017186220 A JP 2017186220A
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- Prior art keywords
- oxide
- transition metal
- metal oxide
- cerium dioxide
- manganese
- 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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- 239000002245 particle Substances 0.000 title claims abstract description 121
- 229910000314 transition metal oxide Inorganic materials 0.000 title claims abstract description 65
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 title claims abstract description 62
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 title claims abstract description 62
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 62
- 239000011572 manganese Substances 0.000 claims abstract description 53
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 claims abstract description 25
- 229910052748 manganese Inorganic materials 0.000 claims abstract description 23
- 229910052742 iron Inorganic materials 0.000 claims abstract description 20
- MWUXSHHQAYIFBG-UHFFFAOYSA-N Nitric oxide Chemical compound O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 abstract description 93
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 abstract description 49
- AMWRITDGCCNYAT-UHFFFAOYSA-L hydroxy(oxo)manganese;manganese Chemical compound [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 abstract description 45
- 239000003054 catalyst Substances 0.000 abstract description 32
- 238000006243 chemical reaction Methods 0.000 abstract description 24
- 238000000746 purification Methods 0.000 abstract description 15
- MGWGWNFMUOTEHG-UHFFFAOYSA-N 4-(3,5-dimethylphenyl)-1,3-thiazol-2-amine Chemical compound CC1=CC(C)=CC(C=2N=C(N)SC=2)=C1 MGWGWNFMUOTEHG-UHFFFAOYSA-N 0.000 abstract description 11
- JCXJVPUVTGWSNB-UHFFFAOYSA-N nitrogen dioxide Inorganic materials O=[N]=O JCXJVPUVTGWSNB-UHFFFAOYSA-N 0.000 abstract description 11
- 229910000510 noble metal Inorganic materials 0.000 abstract description 8
- 230000002708 enhancing effect Effects 0.000 abstract 1
- 230000001747 exhibiting effect Effects 0.000 abstract 1
- 230000001737 promoting effect Effects 0.000 abstract 1
- 239000007789 gas Substances 0.000 description 35
- 235000013980 iron oxide Nutrition 0.000 description 21
- 238000001179 sorption measurement Methods 0.000 description 18
- 230000003197 catalytic effect Effects 0.000 description 14
- 229910044991 metal oxide Inorganic materials 0.000 description 11
- 238000000034 method Methods 0.000 description 11
- 150000004706 metal oxides Chemical class 0.000 description 10
- 230000000052 comparative effect Effects 0.000 description 9
- 238000005259 measurement Methods 0.000 description 9
- 229910002651 NO3 Inorganic materials 0.000 description 8
- 239000013078 crystal Substances 0.000 description 8
- 239000000463 material Substances 0.000 description 8
- 238000005192 partition Methods 0.000 description 8
- 239000000243 solution Substances 0.000 description 8
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 7
- 238000010304 firing Methods 0.000 description 7
- 238000001228 spectrum Methods 0.000 description 7
- 238000002485 combustion reaction Methods 0.000 description 6
- 239000013618 particulate matter Substances 0.000 description 6
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 6
- 239000002994 raw material Substances 0.000 description 6
- 239000004071 soot Substances 0.000 description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- IVMYJDGYRUAWML-UHFFFAOYSA-N cobalt(II) oxide Inorganic materials [Co]=O IVMYJDGYRUAWML-UHFFFAOYSA-N 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 239000006104 solid solution Substances 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 3
- 239000004202 carbamide Substances 0.000 description 3
- 239000011248 coating agent Substances 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- 238000003795 desorption Methods 0.000 description 3
- 238000005470 impregnation Methods 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 229910052697 platinum Inorganic materials 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 238000006722 reduction reaction Methods 0.000 description 3
- XSQUKJJJFZCRTK-UHFFFAOYSA-N urea group Chemical group NC(=O)N XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 239000004215 Carbon black (E152) Substances 0.000 description 2
- GEIAQOFPUVMAGM-UHFFFAOYSA-N Oxozirconium Chemical compound [Zr]=O GEIAQOFPUVMAGM-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 210000004027 cell Anatomy 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 229910001873 dinitrogen Inorganic materials 0.000 description 2
- 238000004993 emission spectroscopy Methods 0.000 description 2
- 229930195733 hydrocarbon Natural products 0.000 description 2
- 150000002430 hydrocarbons Chemical class 0.000 description 2
- 238000007561 laser diffraction method Methods 0.000 description 2
- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Chemical compound O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 description 2
- GEYXPJBPASPPLI-UHFFFAOYSA-N manganese(iii) oxide Chemical compound O=[Mn]O[Mn]=O GEYXPJBPASPPLI-UHFFFAOYSA-N 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 230000001590 oxidative effect Effects 0.000 description 2
- 239000008188 pellet Substances 0.000 description 2
- 230000002093 peripheral effect Effects 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 238000011144 upstream manufacturing Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 238000004438 BET method Methods 0.000 description 1
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 1
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- 238000004998 X ray absorption near edge structure spectroscopy Methods 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
- 229910002091 carbon monoxide Inorganic materials 0.000 description 1
- 229910002090 carbon oxide Inorganic materials 0.000 description 1
- 238000010531 catalytic reduction reaction Methods 0.000 description 1
- 210000002421 cell wall Anatomy 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000007872 degassing Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 239000011491 glass wool Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229910052595 hematite Inorganic materials 0.000 description 1
- 239000011019 hematite Substances 0.000 description 1
- VBMVTYDPPZVILR-UHFFFAOYSA-N iron(2+);oxygen(2-) Chemical class [O-2].[Fe+2] VBMVTYDPPZVILR-UHFFFAOYSA-N 0.000 description 1
- LIKBJVNGSGBSGK-UHFFFAOYSA-N iron(3+);oxygen(2-) Chemical group [O-2].[O-2].[O-2].[Fe+3].[Fe+3] LIKBJVNGSGBSGK-UHFFFAOYSA-N 0.000 description 1
- PPNAOCWZXJOHFK-UHFFFAOYSA-N manganese(2+);oxygen(2-) Chemical class [O-2].[Mn+2] PPNAOCWZXJOHFK-UHFFFAOYSA-N 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- -1 metal oxide nitrate Chemical class 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- GSWAOPJLTADLTN-UHFFFAOYSA-N oxidanimine Chemical compound [O-][NH3+] GSWAOPJLTADLTN-UHFFFAOYSA-N 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 238000001637 plasma atomic emission spectroscopy Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000012495 reaction gas Substances 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
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Abstract
Description
本発明の一実施形態の酸化物含有粒子1は、図1に模式的に示すように、二酸化セリウム粒子2の表面2a及び/または内部に鉄酸化物3a及びマンガン酸化物3bを備えている。ここで、鉄酸化物3a及びマンガン酸化物3bが本発明における遷移金属酸化物に相当する。
本実施形態の酸化物含有粒子1は、種々の使用態様として用いることができる。例えば、図2及び図3に示すような、一方の端面11aから他方の端面11bに向かって流体の流路となる複数のセル12を区画形成する隔壁13を有する円柱状のハニカム構造体14を触媒担体とし、当該ハニカム構造体14の隔壁13の隔壁表面13a等に酸化物含有粒子1を原料の一部として含む表面捕集層15を備えたハニカム触媒体16に使用することができる。これにより、一方の端面11aからハニカム触媒体16の内部に流入した排ガス(図示しない)は、隔壁表面13aに形成された表面捕集層15と接し、当該表面捕集層15の酸化物含有粒子1による触媒効果の影響を受ける。これにより、排ガスが浄化され、他方の端面11bから浄化されたガスが排出される。
既に説明した“含浸法”用い、予め平均粒子径を約3μmに調整した二酸化セリウム粒子の表面に鉄酸化物及びマンガン酸化物の遷移金属酸化物を担持させ、更に大気中で焼成処理を行うことにより酸化物含有粒子を作成した。ここで、遷移金属酸化物の硝酸塩溶液中の鉄成分及びマンガン成分の含有量をそれぞれ変化させ、更に、硝酸塩溶液から取り出した後の二酸化セリウム粒子を焼成する焼成温度を変化させた(300℃または700℃)。これにより、二酸化セリウム粒子の表面等にそれぞれ結晶相や金属酸化物の組成比の異なる遷移金属酸化物を有する酸化物含有粒子の試料(実施例1〜6、及び比較例1〜4)を得た。
上記によって得られた酸化物含有粒子の試料(実施例1〜6、比較例1〜4)に対し、各成分の質量%、二酸化セリウム粒子の平均粒子径、二酸化セリウム粒子の比表面積、遷移金属酸化物の比表面積、結晶相の測定、遷移金属酸化物(Fe2O3,Mn2O3,FeMnO3)の結晶子サイズ、及びFe2+成分及びMn4+成分の比率等の特性を分析及び算出した。以下に、特性の分析及び算出の手法の具体的な方法を示す。
各成分の質量%は、ICP発光分光分析法(Inductivity Coupled Plasma Atomic Emission Spectroscopy)に基づき分析を行うことで算出した。
各粒子の結晶相は、作成された試料に対し、X線回折装置(回転対陰極型X線回折装置:理学電機製、RINT)を用いて測定した。ここで、X線回折測定の条件は、CuKα源、50kV、300mA、2θ=10〜60°とし、得られたX線回折データを市販のX線データ解析ソフトを用いて解析した。
二酸化セリウム粒子の比表面積は、周知のBET法により測定を行った。更に、二酸化セリウム粒子及び遷移金属酸化物の平均粒子径は、レーザー回折法によって算出したメジアン径とした。
遷移金属酸化物の結晶子サイズは、上記2.2のX線回折装置によるX線回折測定によって得られたデータに基づき、これをシェラーの式(τ= Kλ/βcosθ)に当て嵌めることで算出した。ここで、τ:結晶子の平均サイズ、K:形状因子(固体中に含まれる結晶子の大きさと回折パターンのピーク幅との関係を結びつける因子)、λ:X線波長、β:ピーク値全幅(ラジアン単位)、及びθ:ブラッグ角を示している。
X線吸収微細構造(XAFS:X−ray Absorption Fine Structure)スペクトルを測定し、そのXAFSスペクトル中の吸収端近傍構造(XANES)スペクトルを、基準スペクトルを用いて線形フィッティングして算出した。ここで、基準スペクトルは、Mn2+、Mn3+、Mn4+はそれぞれMnO、Mn2O3、及びMnO2のスペクトルとし、Fe2+、Fe3+はそれぞれFeO、Fe2O3のスペクトルとした。
上記1.で得た実施例1〜6及び比較例1〜4の酸化物含有粒子の試料(粉末)を、76MPaの圧力で一軸プレス成形をした。この成形体を目開きが3mmのメッシュで、篩通しした後、1〜2mm程度のペレットを作製した。これを3.00g計量し、NO2変換率の測定試料とした。また、NO吸着量の測定のためには、上記1.で得た酸化物含有粒子の試料(粉末)を、0.1g計量したものを測定試料とした。
NO吸着量は、NOガスを用いた昇温脱離法に基づいて算出した。ここで、NO吸着量の算出のための装置として、AutoChemII(Micromeritis社製)を用いた。更に吸着に用いるガスとして、200pmNO、10%O2、Heの混合ガスを使用した。昇温炉内の反応管内に上記測定試料を載置し、ガス吸着時の温度が250℃となるように設定し、上記ガスを反応管内に導入した。吸着時間は30分とした。吸着完了後、反応管内にHeガスを導入し、昇温速度を10℃/minに設定した条件で、250〜600℃まで昇温を行った。昇温時における脱ガス成分を質量分析計によって計測し、NO脱離量を算出した。係るNO脱離量をNO吸着量とした。
上記2.6によって作成されたペレットを測定試料として、自動車排ガス分析装置(SIGU1000:HORIBA社製)を用いて評価を行った。このとき、昇温炉内の反応管内にグラスウールを敷き上記測定試料を載置し、測定試料が250℃になるまで暖めた。そして、200ppmNO(一酸化窒素)、10%O2(酸素)、及びN2(窒素)の混合ガスを反応ガスとして、反応管内に導入した。このとき、測定試料から排出された排出ガス(出口ガス)を排ガス測定装置(MEXA−6000FT:HORIBA社製)を用いて分析し、それぞれの排出濃度(NO濃度、NO2濃度)を測定した。更に、排出濃度の測定結果に基づいて、NO2変換率を求めた。ここで、NO2変換率は、(1−(NO濃度/(NO濃度+NO2濃度)))により算出される。
Claims (6)
- 二酸化セリウム粒子の表面及び/または内部に、少なくとも鉄成分及びマンガン成分を含む遷移金属酸化物を備える遷移金属酸化物含有二酸化セリウム粒子。
- 前記遷移金属酸化物は、
前記二酸化セリウム粒子よりも小さな粒子径である請求項1に記載の遷移金属酸化物含有二酸化セリウム粒子。 - 前記遷移金属酸化物の含有率は、
15.0質量%〜35.0質量%の範囲である請求項1または2に記載の遷移金属酸化物含有二酸化セリウム粒子。 - 前記遷移金属酸化物は、
前記二酸化セリウム粒子の表面及び/または内部に固溶している請求項1〜3のいずれか一項に記載の遷移金属酸化物含有二酸化セリウム粒子。 - 前記遷移金属酸化物中の前記鉄成分と前記マンガン成分とのモル比率(Fe/Mn比)は、0.2〜20.0の範囲である請求項1〜4のいずれか一項に記載の遷移金属酸化物含有二酸化セリウム粒子。
- 前記遷移金属酸化物は、
全ての前記マンガン成分に占める3価マンガン成分のモル比率は、5.0モル%〜90モル%の範囲である請求項1〜5のいずれか一項に記載の遷移金属酸化物含有二酸化セリウム粒子。
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