JP2013523419A - 低温用、耐水熱性、および耐被毒性のSCR触媒のためのレドックス活性カチオンのホストマトリックスとしてのZrOx、Ce−ZrOx、Ce−Zr−REOx - Google Patents
低温用、耐水熱性、および耐被毒性のSCR触媒のためのレドックス活性カチオンのホストマトリックスとしてのZrOx、Ce−ZrOx、Ce−Zr−REOx Download PDFInfo
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- JP2013523419A JP2013523419A JP2013500374A JP2013500374A JP2013523419A JP 2013523419 A JP2013523419 A JP 2013523419A JP 2013500374 A JP2013500374 A JP 2013500374A JP 2013500374 A JP2013500374 A JP 2013500374A JP 2013523419 A JP2013523419 A JP 2013523419A
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- Prior art keywords
- catalyst
- zeolite
- nitrogen
- slurry
- lattice
- Prior art date
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- 239000003054 catalyst Substances 0.000 title claims abstract description 141
- 150000001768 cations Chemical class 0.000 title claims abstract description 73
- 229910003134 ZrOx Inorganic materials 0.000 title description 12
- 231100000331 toxic Toxicity 0.000 title description 4
- 230000002588 toxic effect Effects 0.000 title description 4
- MWUXSHHQAYIFBG-UHFFFAOYSA-N nitrogen oxide Inorganic materials O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 claims abstract description 279
- 238000000034 method Methods 0.000 claims abstract description 139
- 239000000463 material Substances 0.000 claims abstract description 108
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 33
- 238000004458 analytical method Methods 0.000 claims abstract description 16
- 239000006104 solid solution Substances 0.000 claims abstract description 12
- QWDUNBOWGVRUCG-UHFFFAOYSA-N n-(4-chloro-2-nitrophenyl)acetamide Chemical compound CC(=O)NC1=CC=C(Cl)C=C1[N+]([O-])=O QWDUNBOWGVRUCG-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000010457 zeolite Substances 0.000 claims description 92
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 claims description 77
- 229910021536 Zeolite Inorganic materials 0.000 claims description 76
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 61
- 239000000203 mixture Substances 0.000 claims description 58
- 238000006243 chemical reaction Methods 0.000 claims description 54
- 229910052751 metal Inorganic materials 0.000 claims description 38
- 239000002184 metal Substances 0.000 claims description 38
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- 239000010949 copper Substances 0.000 claims description 28
- 239000002019 doping agent Substances 0.000 claims description 28
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 28
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 claims description 28
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- 238000002441 X-ray diffraction Methods 0.000 claims description 14
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 14
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- UNYSKUBLZGJSLV-UHFFFAOYSA-L calcium;1,3,5,2,4,6$l^{2}-trioxadisilaluminane 2,4-dioxide;dihydroxide;hexahydrate Chemical compound O.O.O.O.O.O.[OH-].[OH-].[Ca+2].O=[Si]1O[Al]O[Si](=O)O1.O=[Si]1O[Al]O[Si](=O)O1 UNYSKUBLZGJSLV-UHFFFAOYSA-L 0.000 claims description 9
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- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 33
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 17
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- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 description 1
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- 150000007522 mineralic acids Chemical class 0.000 description 1
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- 239000011733 molybdenum Substances 0.000 description 1
- 229910000476 molybdenum oxide Inorganic materials 0.000 description 1
- 229910052680 mordenite Inorganic materials 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 150000007524 organic acids Chemical class 0.000 description 1
- 235000005985 organic acids Nutrition 0.000 description 1
- 150000007530 organic bases Chemical class 0.000 description 1
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 description 1
- PQQKPALAQIIWST-UHFFFAOYSA-N oxomolybdenum Chemical compound [Mo]=O PQQKPALAQIIWST-UHFFFAOYSA-N 0.000 description 1
- 239000003002 pH adjusting agent Substances 0.000 description 1
- 230000002688 persistence Effects 0.000 description 1
- 230000002085 persistent effect Effects 0.000 description 1
- 238000004375 physisorption Methods 0.000 description 1
- 239000005373 porous glass Substances 0.000 description 1
- 238000010248 power generation Methods 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 238000009790 rate-determining step (RDS) Methods 0.000 description 1
- 230000002468 redox effect Effects 0.000 description 1
- 238000005067 remediation Methods 0.000 description 1
- 238000001175 rotational moulding Methods 0.000 description 1
- 229910052707 ruthenium Inorganic materials 0.000 description 1
- KZUNJOHGWZRPMI-UHFFFAOYSA-N samarium atom Chemical compound [Sm] KZUNJOHGWZRPMI-UHFFFAOYSA-N 0.000 description 1
- 229910052706 scandium Inorganic materials 0.000 description 1
- SIXSYDAISGFNSX-UHFFFAOYSA-N scandium atom Chemical compound [Sc] SIXSYDAISGFNSX-UHFFFAOYSA-N 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
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- 230000007704 transition Effects 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
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- 239000010455 vermiculite Substances 0.000 description 1
- 235000019354 vermiculite Nutrition 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- NAWDYIZEMPQZHO-UHFFFAOYSA-N ytterbium Chemical compound [Yb] NAWDYIZEMPQZHO-UHFFFAOYSA-N 0.000 description 1
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Abstract
Description
N2+O・→NO+N・ (1)
N・+O2→NO+O・ (2)
示されたように、酸化窒素は、生物に直接毒性があり(P.E.Morrow J.Toxicol Environ Health 13(2−3),(1984),205−27)、それに加えて、NOxは、いくつかの環境汚染源に直接寄与したり、それらの間接的要因になったりする。したがって、酸化窒素は、酸性雨の形成に直接関与するだけでなく、人の健康への著しい悪影響に相関付けられてきた光化学スモッグおよびオゾンの生成過程における反応剤でもある(M.V.Twigg,Applied Catalysis B,vol.70,(2007),2)。そのため、ガソリンおよびディーゼルの両方の内燃機関の排気からのそのような化合物の排出を規制すべく、ますます厳しくなる法的規制が導入されてきた。たとえば、Euro5またはEuro6[Regulation(EC) No715/2007 of the European Parliament and of the Council,20 Jun.2007、Official Journal of the European Union L171/1、また、Twigg,Applied Catalysis B,vol.70,(2007),p2−25およびR.M.Heck,R.J.Farrauto Applied Catalysis A vol.221,(2001),p443−457ならびにそれらの中の参照文献も参照されたい]。
(4) 4NO+4NH3+O2→4N2+6H2O 標準的/「遅い」SCR
(5) 3NO2+4NH3→(7/2)N2+6H2O NO2のみのSCR
(6) NO+NO2+2NH3→2N2+3H2O 「速い」SCR
(7) 4NH3+3O2→2N2+6H2O N2への寄生NH3酸化
(8) 4NH3+5O2→4NO+6H2O NOへの寄生NH3酸化
(9) 2NH3+2O2→N2O+3H2O N2Oへの寄生NH3酸化
主要反応機構は、式(3)で表される。しかしながら、実用条件下では、NOxの約50%がNO2として存在するNO/NO2混合物の反応でNH3によるNOx転化(式4)の速度が最大になることが繰返し実証されてきた(非特許文献1およびその中の参照文献)。さらに、NH3とNO2との反応が起こることが知られているが(式5)、速度論的に支配的でないため、NO2濃度が約50%を超えると、触媒活性および総括速度が付随的に減少する(非特許文献2)。しかしながら、反応速度はまた、反応温度、この特定例では使用される触媒の種類、ならびに実際にはガス流中の反応性被毒物質の存在およびそこで利用されるさまざまな触媒配合物の相対耐被毒性に依存して大きく変化するであろうことを常に強調しておかなければならない。
(b)追加の相の形成を伴わずに前記格子構造内に分散された触媒活性カチオンと、ここで、純相格子構造は、ジルコニウムの酸化物から誘導されるものとする、
を含む卑金属触媒の存在下で前記酸化窒素を窒素含有還元剤に接触させる、窒素酸化物から窒素への転化方法を説明する。
OS1 CeO2 31.99 ZrO2 50.9 La2O3 4.9 Y2O3 4.88 Fe2O3 7.33
OS2 CeO2 44.75 ZrO2 36.28 Nd2O3 9.87 Pr6O11 4.48 Nb2O5 4.62
OS3 CeO2 44.72 ZrO2 35.33 Nd2O3 9.68 Pr6O11 4.59 Nb2O5 4.72 Fe2O3 0.96
OS4 CeO2 31.76 ZrO2 54.79 Y2O3 6.44 Nb2O5 7.01
OS5 CeO2 44.33 ZrO2 38.06 La2O3 9.77 Pr6O11 4.66 Fe2O3 3.18
OS6 CeO2 44.4 ZrO2 35.36 La2O3 9.77 Pr6O11 4.74 Nb2O5 4.58 Fe2O3 1.15
OS7 CeO2 38.75 ZrO2 47.7 La2O3 4.82 Pr6O11 4.72 CuO 4
OS8 CeO2 32.07 ZrO2 54.1 Y2O3 6.39 Nb2O5 7.44
OS9 CeO2 36.07 ZrO2 54.19 Y2O3 4.87 Nb2O5 4.87
OS10 CeO2 32.26 ZrO2 51.95 La2O3 2.05 Y2O3 6.29 Nb2O5 7.45
OS11 CeO2 44 ZrO2 39.5 La2O3 9.5 Pr6O11 4.5 CaO 2.5
OS12 CeO2 31.5 ZrO2 52.3 La2O3 5 Y2O3 5 SrO 5
OS13 CeO2 30.22 ZrO2 52.16 Y2O3 7.84 Pr6O11 2.05 Nb2O5 7.73
OS14 CeO2 30 ZrO2 48.4 Y2O3 9.85 Pr6O11 2.02 Nb2O5 9.73
OS15 CeO2 30.14 ZrO2 54.16 Y2O3 7.85 Nb2O5 7.85
OS16 CeO2 31.5 ZrO2 58.6 La2O3 4.9 Y2O3 5
OS17 CeO2 31 ZrO2 57 Y2O3 5 La2O3 3 Pr6O11 3 SrO 1
OS18 CeO2 31 ZrO2 58 Y2O3 5 La2O3 5 SrO 1
OS19 CeO2 31 ZrO2 58 Y2O3 5 Pr6O11 5 SrO 1
ウォッシュコートの定義はg/in3単位であり、これらの研究で使用した市販の対照触媒はすべて、5%CuMFI40に基づくものである。
0.5 Al2O3 1.5 OS1
0.5 Al2O3 1.5 OS2
0.5 Al2O3 1.5 OS3
図2:
1.3 Al2O3 2.7 OS4
1.3 Al2O3 2.7 OS5
1.3 Al2O3 2.7 OS6
図3:
1.3 Al2O3 2.7 OS4
図4:
0.5 Al2O3 1 3% Fe−MFI(27) 2 OS7
1.1 Al2O3 0.5 3% Fe−MFI(27) 2 OS7
1.1 Al2O3 2.5 OS7
図5:
1.1 Al2O3 1パス|2.5 OS8 2パス
1.1 Al2O3 1パス|2.5 OS9 2パス
1.1 Al2O3 1パス|2.5 OS10 2パス
図6:
1.1 4% La2O3−−Al2O3 1パス|2.5 OS11 2パス
1.5 4% La2O3−−Al2O3 1パス|2.5 OS11 2パス
1.5 4% La2O3−−Al2O3 1パス|2.5 OS12 2パス
図7:
1.5 4% La2O3−−Al2O3 1パス|0.5 MFI(40) 2 OS12 2パス
1.5 4% La2O3−−Al2O3 1パス|0.5 MFI(40) 2 OS12 2パス|0.225 Cu(NH3OH)4
1.5 4% La2O3−−Al2O3 1パス|2.5 OS12 2パス|0.225 Cu(NH3OH)4
図8:
1.1 Al2O3 1パス|2.5 OS14 2パス
1.1 Al2O3 1パス|2.5 OS13 2パス
1.1 Al2O3 1パス|2.5 OS15 2パス
図9: a)300℃およびb)400℃での過渡SCR応答のSGB分析
0.5 Al2O3 1.5 5% CuMFI(40) 1.5 OS8
図10: 温度ランプ時のNH3「プルーム」形成のSGB分析。
表1: エンジンダイノ試験の詳細
表2: OS4、OS5、およびOS6のXRD相分析
表3: OS11およびOS12のXRD相分析
表4: SGB分析
1.1 Al2O3 1パス|2.5 OS9 2パス
0.5 Al2O3 1.5 5% CuMFI(40) 1.5 OS8
表5: 660℃で50時間のダイノエージングを行った後の市販のゼオライトSCRと対比されたOS材料のエンジンダイノ性能に及ぼすMHSVおよびDOC(w)の影響
1.1 Al2O3 1パス|2.5 OS9 2パス
0.5 Al2O3 1.5 5% CuMFI(40) 1.5 OS8
表6: 660℃で50時間のダイノエージングを行った後のWで機能強化されたOS材料のエンジンダイノ性能に及ぼすMHSVおよびDOCの存在の影響
0.35 Al2O3 0.2889W 2.6OS8
0.35 Al2O3 0.2889W 1.7334OS8 0.8666OS16
0.35 Al2O3 0.2889W 1.7334OS16 0.8666OS8
1.1 Al2O3 1パス|2.5 OS8 2パス
表7: 660℃で50時間のダイノエージングを行った後のWで機能強化された二重OS材料のエンジンダイノ性能に及ぼすタングステン機能強化、MHSV、およびDOCの存在の影響
0.35 Al2O3 0.2889W 2.6OS17
0.35 Al2O3 0.2889W 2.6OS8
0.35 Al2O3 0.2889W 2.6OS18
0.35 Al2O3 0.2889W 2.6OS19
例示的実施形態を参照しながら本発明を以上で説明してきたが、本発明の範囲および一般原理から逸脱することなく、種々の変更を加えることが可能であり、等価物をその要素の代わりに使用可能であることは当業者であればわかるであろう。それに加えて、特定の状況または材料に適合するように本発明の教示に対してその本質的な範囲から逸脱することなく多くの変更を加えることが可能である。したがって、本発明は、本発明の実施に利用可能と考えられる最良の形態として開示された特定の実施形態に限定されるものではなく、本発明は、添付の特許請求の範囲に包含されるすべての実施形態を含むものとする。
(b)前記格子構造内に分散された触媒活性カチオンと、
を含む卑金属酸化物触媒の存在下で窒素酸化物を窒素含有還元剤に接触させることによる、窒素酸化物から窒素への転化方法。
(b)前記格子構造内(with)に分散された触媒活性カチオンと、ここで、触媒的分散カチオンは、元素周期表の遷移金属系列、アルカリ土類金属族、アルカリ金属族、およびそれらの混合物よりなる群から選択されるものとする、
よりなる触媒と共に任意選択の低ゼオライト/ゼオタイプ含有分を有する不均一卑金属触媒。
Claims (16)
- 窒素酸化物から窒素への転化方法であって、
(a)従来の粉末X線回折(XRD)法により決定したときに相純度>95%の結晶格子構造と、
(b)追加の相の形成を伴わずに前記格子構造内に分散された触媒活性カチオンと、ここで、前記純相格子構造は、ジルコニウムの酸化物から誘導されるものとする、
を含む卑金属酸化物触媒の存在下で前記窒素酸化物を窒素含有還元剤に接触させることによる、窒素酸化物から窒素への転化方法。 - 前記純相格子構造がセリウム−ジルコニウムの酸化物固溶体から誘導される、請求項1に記載の方法。
- 前記活性分散カチオンが、元素周期表の遷移金属系列、元素周期表のアルカリ土類金属族、および元素周期表のアルカリ金属族よりなる群の1種以上の元素から選択される、請求項1〜2のいずれか1項に記載の方法。
- 前記活性分散カチオンが、Cu、Fe、Nb、Ta、W、およびそれらの混合物よりなる群から選択される、請求項1〜3のいずれか1項に記載の方法。
- 前記温度が約150℃〜約700℃である、請求項1〜4のいずれか1項に記載の方法。
- 窒素酸化物から窒素への前記転化が過剰の酸素の条件下で行われる、請求項1〜5のいずれか1項に記載の方法。
- 窒素含有還元剤源が、触媒入口で0.5〜2の効果的なNH3:NOx比(α比)が得られるように導入される、請求項1〜6のいずれか1項に記載の方法。
- 前記触媒入口で記録されるNO:NO2比が体積基準で1:0〜1:3である、請求項1〜7のいずれか1項に記載の方法。
- 酸化触媒が、NO2富化排気ガスの発生を可能にするために前記卑金属酸化物(SCR)触媒の前に利用される、請求項8に記載の方法。
- 従来のX線回折(XRD)法による相分析で実質的に純相の材料(>95%)であることが明らかになり、バルク金属酸化物ドーパント相が<5%で記録され、かつ線の広がりにより決定したときに/Scherrer式により決定したときにドーパント金属酸化物粒子サイズが約30Å〜約100Åになるように、触媒としての前記触媒活性カチオンドープ格子が、追加の相の形成を伴わずに純相結晶格子構造への触媒活性カチオンの組込みを含む、請求項1〜9のいずれか1項に記載の方法。
- 前記格子構造中にドープされる前記触媒活性カチオンが、前記触媒の全質量を基準にして約1wt%〜7.5%である、請求項1〜10のいずれか1項に記載の方法。
- 前記触媒活性カチオンドープ格子材料が、共沈を介して直接合成により作製される、請求項1〜11のいずれか1項に記載の方法。
- 前記触媒が、ゼオライト/ゼオタイプまたは金属交換ゼオライト/ゼオタイプに基づく共触媒を追加的に含有する、請求項1〜12のいずれか1項に記載の方法。
- 前記ゼオライト/ゼオタイプまたは金属交換ゼオライト/ゼオタイプが、全触媒質量の約1wt%〜約35wt%である、請求項1〜13のいずれか1項に記載の方法。
- 前記ゼオライト/ゼオタイプまたは金属交換ゼオライト/ゼオタイプが、ZSM5、ゼオライトβ、チャバザイト、SAPO−34、8環細孔開口構造を含有する構造により特性付けられるゼオライト、およびそれらの混合物よりなる群から選択される、請求項1〜14のいずれか1項に記載の方法。
- 前記金属交換ゼオライト/ゼオタイプで利用される金属が、銅、鉄、およびそれらの混合物よりなる群から選択される、請求項1〜15のいずれか1項に記載の方法。
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JP2013544628A (ja) * | 2010-09-29 | 2013-12-19 | ロデイア・オペラシヨン | 酸化セリウム及び酸化ニオブを含む組成物が触媒として使用される、窒素酸化物(NOx)を含む気体を処理する方法 |
JP2015174023A (ja) * | 2014-03-14 | 2015-10-05 | トヨタ自動車株式会社 | 排ガス浄化用触媒 |
JPWO2017051459A1 (ja) * | 2015-09-24 | 2018-08-30 | 本田技研工業株式会社 | 排気浄化フィルタ |
US10677124B2 (en) | 2015-09-24 | 2020-06-09 | Honda Motor Co., Ltd. | Exhaust purification filter |
US10704440B2 (en) | 2015-09-24 | 2020-07-07 | Honda Motor Co., Ltd. | Exhaust purification system of internal combustion engine |
JP2019072696A (ja) * | 2017-10-19 | 2019-05-16 | 株式会社豊田中央研究所 | 酸素貯蔵材料及びその製造方法 |
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WO2011116907A3 (en) | 2012-03-15 |
US8017097B1 (en) | 2011-09-13 |
EP2552831A2 (en) | 2013-02-06 |
CN102781572A (zh) | 2012-11-14 |
US20110236282A1 (en) | 2011-09-29 |
WO2011116907A2 (en) | 2011-09-29 |
JP5841123B2 (ja) | 2016-01-13 |
BR112012024344A2 (pt) | 2017-07-18 |
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