JP5438772B2 - 燃料添加剤含有格子操作二酸化セリウムナノ粒子 - Google Patents
燃料添加剤含有格子操作二酸化セリウムナノ粒子 Download PDFInfo
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- JP5438772B2 JP5438772B2 JP2011542092A JP2011542092A JP5438772B2 JP 5438772 B2 JP5438772 B2 JP 5438772B2 JP 2011542092 A JP2011542092 A JP 2011542092A JP 2011542092 A JP2011542092 A JP 2011542092A JP 5438772 B2 JP5438772 B2 JP 5438772B2
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- Prior art keywords
- cerium
- cerium dioxide
- nanoparticles
- transition metal
- ions
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- 239000002816 fuel additive Substances 0.000 title description 19
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Description
本願は、国際出願第PCT/US07/077545号の「METHOD OF PREPARING CERIUM DIOXIDE NANOPARTICLES」及び国際出願第PCT/US07/077535号の「CERIUM DIOXIDE NANOPARTICLE−CONTAINING FUEL ADDITIVE」(共に2007年9月4日に出願)に関する。これらの出願は、仮出願番号第60/824514号の「CERIUM−CONTAINING FUEL ADDITIVE」(2006年9月5日に出願)、仮出願番号第60/911159号の「REVERSE MICELLAR FUEL ADDITIVE COMPOSITION(2007年4月11日に出願)及び仮出願番号第60/938314号の「REVERSE MICELLAR FUEL ADDITIVE COMPOSITION」(2007年5月16日に出願)の優先権の利益を主張するものである。これらの全ての出願の開示は、参照により本願に組み込まれる。
〔式1〕
CeO2← →CeO2-X+x/2O2
CO+H2O → CO2+H2
によって、燃料の燃焼で発生する有毒な排ガスを削減する触媒としての役割を果たすだけではなく、ディーゼルエンジンで典型的に使用される微粒子トラップに蓄積される微粒子の完全燃焼も促進する。
(H2O)p[CeO(A)2(AH)n]m
(式中、ラジカルAは同一又は異なり、それぞれ1より大きいpKaを有する有機酸素酸AHのアニオンであり、pは0〜5の整数であり、nは0〜2の数字であり、mは1〜12の整数である)を有する酸化セリウム(IV)化合物を開示している。この有機酸素酸は好ましくはカルボン酸であり、より好ましくはC2〜C20モノカルボン酸又はC4〜C12ジカルボン酸である。セリウム含有化合物は、炭化水素燃料の燃焼のための触媒として利用可能である。
Ce(M)x(OH)y(NO3)2
(式中、Mはアルカリ金属又は第4級アンモニウムラジカルを表し、xは0.01〜0.2であり、yはy=4−z+xとなるようなものであり、zは0.4〜0.7である)に対応するセリウム(IV)化合物が開示されている。セリウム(IV)化合物のコロイド分散系を調製するためのプロセスでは、約1〜約60nm、適切には約1〜約10nm、望ましくは約3〜8nmの流体力学的直径を有する粒子が製造される。
〔式2〕(0057)
log Δa=−0.4763 logD−1.5029
〔式3〕(0086)
AgNO3+NaCl → AgCl+NaNO3
〔式4〕
RO(CH2CH2O)nCHR1CO2Y (Ia)
〔式5〕
XO2C(CR2)PCO2Z (Ib)
〔式6〕
Ce(NO3)3(6H2O)+2NH4OH → Ce(OH)2NO3+2NH4NO3+6H2O (3a)
〔式7〕
2Ce(OH)2NO3+H2O2 → 2CeO2+2HNO3+2H2O (3b)
〔式8〕
Ce(NO3)3(6H2O)+3NH4OH → Ce(OH)3+3NH4NO3+6H2O (4a)
〔式9〕
2Ce(OH)3+H2O2 → 2CeO2+4H2O (4b)
〔式10〕
R3(OCH2CH2)mOH (Ic)
〔式11〕
RO(CH2CH2O)aCHR1CO2Y (Ia)
(式中、Rは水素、置換若しくは非置換アルキル基又は置換若しくは非置換芳香族基を表し、R1は水素又はアルキル基を表し、YはH又は対イオンを表し、nは0〜5である)の界面活性剤を含み得る。好ましくは、Rは置換又は非置換アルキル基を表し、R1は水素を表し、Yは水素を表し、nは2である。
〔式12〕
XO2C(CR2)PCO2Z (Ib)
(式中、各R2は独立して水素、置換若しくは非置換アルキル基又は置換若しくは非置換芳香族基を表し、X及びZは独立してH又は対イオンを表し、pは1又は2である)のジカルボキシレートを含む。
〔式13〕
R3(OCH2CH2)mOH (Ic)
(式中、R3は置換又は非置換アルキル基を表し、mは1〜8の整数である)の化合物を含み得る。
〔式14〕
R3Φ(OCH2CH2)mOH (Id)
(式中、R3は置換又は非置換アルキル基を表し、Φは芳香族基であり、mは4〜6の整数である)の化合物も含み得る。
3リットルの丸底ステンレススチール反応器槽に、1.267リットルの蒸留水、続いて100mlのCe(NO3)3・6H2O溶液(600g/リットルのCe(NO3)3・6H2O)を加えた。溶液は透明であり、20℃でpH4.2を有した。続いて、30.5gの2−[2−(2−メトキシエトキシ)エトキシ]酢酸(MEEA)を、槽に加えた。溶液は透明のままであり、pHは20℃で2.8であった。高せん断ミキサー(Silverson Machines製。反応物が蠕動性チュービングポンプによってミキサーブレード内に直接導入可能なように改造されたコロイドミル)を反応器槽内に下降させ、ミキサーヘッドを反応器槽の底部の少し上に位置決めした。ミキサーを5000rpmに設定し、8.0gの30%H2O2を反応器槽に加えた。次に、40mlにまで希釈された16mlの28〜30%NH4OHを、ミキサーヘッドにより約12秒で反応器槽内にポンプ輸送した。最初は透明だった溶液が、橙色/褐色に変化した。高せん断ミキサーを取り外し、反応器槽を、温度制御ウォータージャケットにまで移動し、R−100プロペラを備えたミキサーを使用して、溶液を450rpmで撹拌した。反応器内にNH4OHをポンプ輸送後3分で、pHは25℃で3.9であった。次の25分に亘って、反応器槽の温度を70℃にまで上昇させた。この時、pHは3.9であった。溶液温度を20分間に亘って70℃で維持した。この間、溶液の色は橙褐色から透明な暗黄色に変化した。pHは70℃で3.6であった。次の25分に亘って温度を25℃にまで低下させた。この時、pHは25℃で4.2であった。動的光散乱法による粒子サイズ分析は、二酸化セリウム強度加重流体力学的直径6nmを示した。次に、分散系を、導電率3mS/cmにまでダイアフィルトレーションに供し、約10倍、CeO2粒子で公称1モルにまで濃縮した。
この沈殿は実施例1に倣って行われる。ただし、EDTAと乳酸との安定剤の組み合わせ(比は20:80。76.4gのEDTA二ナトリウム塩及び74.0gの85%乳酸)をMEEA安定剤の代わりに使用する。図3Aは高倍率TEM画像であり、実質的に5nm未満であり1.1±0.3nmと推定される結晶粒サイズを示す。図3Bは代表的な沈殿サンプルの電子回折パターンである。図3Cには表1が含まれ、表では様々な回折リング{311}、{220}、{200}、{111}の強度が立方晶CeO2、立方晶及び六方晶Ce2O3、Ce(OH)3のフレームワーク内で分析される。明らかに、晶癖を含めた分析済みのリング強度のパーセント偏差は、CeO2の立方晶ホタル石型構造に関して最小限であったことから、この結晶粒直径でのこの多形体の存在が証明される。
3リットルの丸底ステンレススチール反応器槽に、1117グラムの蒸留水を加えた。標準Rv100プロペラを反応器槽内に下降させ、ミキサーヘッドを反応器槽の底部の少し上に位置決めした。ミキサーを700rpmに設定し、反応器の温度を約70℃にした。次に、59.8グラム(98%)のメトキシ酢酸を反応器に加えた。120.0グラムのCe(NO3)3・6H2Oを含有する250mlの溶液を反応器内に、69.5グラム(28〜30%)の水酸化アンモニウムを含有する溶液と同時にポンプ輸送することによって、ダブルジェット沈殿を5分間に亘って行った。反応器にすすぎ用の蒸留水を流すことによって、反応物供給管から残留物質が除去された。次に、10.2グラムの50%非安定化過酸化水素を反応器及びその内容物に40秒で加えた。最初は、反応混合物は、不透明で暗橙褐色のpH6〜7の液体であった。この反応混合物を更に60分間に亘って加熱し、この間にpHは4.25に低下し(反応(3a)及び(3b)によるヒドロニウムイオンの放出と合致する)、混合物は透明な黄橙色になった。反応混合物を20℃にまで冷却し、導電率3mS/cmにまでダイアフィルトレーションに供することによって過剰な水及び未反応材料を除去した。これによって分散系は約10倍又はCeO2粒子で公称1モルにまで濃縮された。透過型電子顕微鏡分析による粒径分布分析によって(図4)、平均粒子サイズが2.2nmであり、粒径分布は変動係数COV(標準偏差を平均直径で割ったもの)23%を有すると判明した。計算された収率は62.9%であった。
実施例3の条件を繰り返した。ただし、硝酸セリウム溶液は、108.0グラムの硝酸セリウム六水和物及び6.42グラムのCe(NO3)3・2.5H2Oを含有していた。これらの金属塩を別々に溶解し、次にそれらを混合することによって250mlの溶液を生成した。反応は、実施例3に記載されるようにして進行した。ただし、過酸化水素は、セリウム及びアンモニアが添加されてから40秒で添加された。透過型電子顕微鏡分析による粒径分布分析によって(図5)、平均粒子サイズが2.5nmであり、粒径分布は変動係数COV(標準偏差を平均直径で割ったもの)25%を有すると判明した。2峰性の分布が存在しないことに留意すること。2次ピークは、CuがCeO2格子には取り込まれず、別個のCu2O3として存在することを示すと考えられる。
実施例4の条件を繰り返した。ただし、金属塩溶液は、108.0グラムの硝酸セリウム六水和物及び11.16グラムのFe(NO3)3・9H2Oを含有していた。これらの金属塩を別々に溶解し、次にそれらを混合することによって250mlの溶液を生成した。反応は、実施例4に記載されるようにして進行した。沈殿した粒子のTEM画像(図6A)及び透過型電子顕微鏡分析による粒径分布分析によって(図6B)、平均粒子サイズが2.2±0.7nmであり、粒径分布は変動係数COV(標準偏差を平均直径で割ったもの)32%を有すると判明した。計算された収率は55.1%であった。
実施例4の条件を繰り返した。ただし、金属塩溶液は、101.89グラムの硝酸セリウム六水和物及び9.57グラムのZrO(NO3)2・6H2Oを含有していた。これらの金属塩を別々に溶解し、次にそれらを混合することによって250mlの溶液を生成した。反応は、実施例4に記載されるようにして進行した。ただし、反応は85℃で行われた。透過型電子顕微鏡分析による粒径分布分析によって(図7A)、平均粒子サイズが2.4±0.7nmであり、粒径分布は変動係数COV(標準偏差を平均直径で割ったもの)29%を有すると判明した。誘導結合プラズマ原子発光分光法によって、Ce0.82Zr0.18O1.91の化学量論比が判明し、ZrO2のCeO2への相対不溶性を考えると、これはより高いZr含有量(18%対15%)の説明となる。
実施例4の条件を繰り返した。ただし、金属塩溶液は、84.0グラムの硝酸セリウム六水和物、11.16グラムのFe(NO3)3・9H2O及び12.76グラムのZrO(NO3)2・6H2Oを含有していた。これらの金属塩を別々に溶解し、次にそれらを混合することによって250mlの溶液を生成した。反応は、実施例4に記載されるようにして進行した。ただし、反応は85℃で行われ、過酸化水素溶液(50%)は20.4gに増量され、10分で添加された。粒子のTEM画像(図8A)及び透過型電子顕微鏡分析による粒径分布分析によって(図8B)、平均粒子サイズが2.2±0.6nmであり、粒径分布は変動係数COV(標準偏差を平均直径で割ったもの)27%を有すると判明した。ここでもまた、単分散、単峰性の分布が、ZrO2及びFe2O3結晶粒が別々に再核形成されるのではなく共に取り込まれる概念を裏付けている。計算された収率は78%であった。誘導結合プラズマ原子発光分光法によって、Ce0.69Fe0.14Zr0.17O0.915の化学量論比が判明した。ここでもまた、公称量に対して相対的により濃縮されたFe及びZrは、その水酸化物前駆体の水酸化セリウムのものより高い不溶性を反映している。図8Cも、遷移金属非含有CeO2と比較したこのサンプル(上の曲線)の粉末X線回折パターンである。32度2θでのピーク(矢印で示される)の欠如は、遊離のZrO2がないことを意味する。すなわち、セリウム格子に全て取り込まれている。また、50、52度2θでのピークの欠如は、Fe2O3が別箇に存在しないことを示す(すなわち、Feのセリウム格子への取り込み)。大きな2θ散乱角でのより大きな2θへのシフトに留意すること。これは格子(nλ/2d=sinθ)の歪み又は収縮を示し、置き換わるCe4+(0.97Å)に対するFe3+(0.78Å)及びZr4+(0.84Å)のより小さいイオン半径に合致している。このため、遷移金属がCeO2格子に取り込まれ、純粋なZrO2及びFe2O3ナノ粒子が別箇に存在しないと発明者は結論づけた。単峰性の粒径分布もこの結論を裏付けている。
実施例7aの条件に倣った。しかしながら、適切な金属含有塩溶液を使用して、鉄又はジルコニウムの量を調節して記載の公称化学量論比を得た。一方、硝酸セリウム六水和物全体が、上昇した濃度の鉄又はジルコニウム遷移金属に対応するために還元された。
Claims (14)
- 少なくとも1種の遷移金属(M)を含有する格子操作結晶性二酸化セリウムナノ粒子を形成するためのプロセスであって、
(a)3価のセリウムイオンの供給源、1種以上の遷移金属イオン(M)の供給源、水酸化物イオンの供給源、少なくとも1種のナノ粒子安定剤及び酸化剤を含む水性反応混合物を25℃より高くから95℃までの初期温度で得て、
(b)前記混合物を機械的にせん断し、また穿孔スクリーンを通過させることによって水酸化セリウムナノ粒子の均質に分布した懸濁液を生成し、
(c)3価のセリウムイオンを4価のセリウムイオンに酸化するのに効果的な温度条件にすることによって、遷移金属含有二酸化セリウムナノ粒子Ce1-xMxO2(式中、xは0.3〜0.8の値を有する)を含む生成物流を生成することを含み、前記温度条件が50〜100℃の温度を含み、前記ナノ粒子が、結晶性立方晶ホタル石型構造、1〜10nmの平均流体力学的直径及び1〜4nmの幾何学的直径を有することを特徴とするプロセス。 - 前記機械的せん断がコロイドミルで行われる、請求項1に記載のプロセス。
- 3価のセリウムイオンを4価のセリウムイオンに酸化するのに効果的な前記温度条件が60〜90℃の温度を含む、請求項1に記載のプロセス。
- 前記イオンの供給源が、前記反応混合物に、前記機械的せん断中に同時に又は順次導入される、請求項1に記載のプロセス。
- 前記二酸化セリウムナノ粒子が、6nmの平均流体力学的直径を有する、請求項1に記載のプロセス。
- 請求項1に記載のプロセスによって形成された安定化された格子操作遷移金属含有結晶性二酸化セリウムナノ粒子Ce1-xMxO2 (式中、xは0.3〜0.8の値を有する)を含有する均質な分散系を生成するためのプロセスであって、
(a)立方晶ホタル石型構造を有する安定化された遷移金属ドープ二酸化セリウムナノ粒子Ce1-xMxO2を含む水性混合物を得て、前記ナノ粒子が、1〜10nmの平均流体力学的直径及び4nm未満の幾何学的直径を有し、
(b)前記安定化された遷移金属含有二酸化セリウムナノ粒子を含む前記水性混合物を濃縮することによって水性濃縮物を生成し、
(c)前記水性濃縮物から全ての水を除去することによって、前記安定化された遷移金属含有二酸化セリウムナノ粒子の水を含有しない濃縮物を生成し、
(d)有機希釈剤を前記水を含有しない濃縮物に添加することによって、前記安定化された遷移金属含有二酸化セリウムナノ粒子の有機濃縮物を生成し、
(e)前記有機濃縮物を、無極性媒質の存在下、界面活性剤と混合することによって、安定化された遷移金属含有結晶性二酸化セリウムナノ粒子Ce1-xMxO2を含有する均質な分散系を形成することを含むことを特徴とするプロセス。 - 前記遷移金属含有二酸化セリウムナノ粒子Ce1-xMxO2における前記遷移金属Mが、Fe、Mn、Cr、Ni、W、Co、V、Cu、Zr、Y、Mo及びこれらの組み合わせから成る群から選択される、請求項6に記載のプロセス。
- xが、0.30〜0.80の値を有する、請求項7に記載のプロセス。
- xが、0.40〜0.60の値を有する、請求項8に記載のプロセス。
- 前記遷移金属MがZr又はYを含む、請求項7に記載のプロセス。
- 前記遷移金属Mが更にFeを含む、請求項10に記載のプロセス。
- 前記有機希釈剤がグリコールエーテルを含む、請求項6に記載のプロセス。
- 内燃機関排気系の触媒コンバータ用ウォッシュコートであって、請求項6に従って形成された安定化された遷移金属含有結晶性二酸化セリウムナノ粒子を含有する均質な分散系を使用して形成されることを特徴とするウォッシュコート。
- 還元反応又は酸化反応の加速に効果的な触媒であって、請求項6に従って形成された安定化された遷移金属含有結晶性二酸化セリウムナノ粒子を含有する均質な分散系を使用して生成されることを特徴とする触媒。
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JPS5945925A (ja) * | 1982-06-11 | 1984-03-15 | ロ−ヌ−プ−ラン・スペシアリテ・シミ−ク | コロイド状酸化セリウム分散液の製造方法 |
FR2741281B1 (fr) * | 1995-11-22 | 1998-02-13 | Rhone Poulenc Chimie | Sol organique comportant au moins un compose oxygene de terre(s) rare(s), procede de synthese du dit sol et utilisation du dit sol pour la catalyse |
US6133194A (en) * | 1997-04-21 | 2000-10-17 | Rhodia Rare Earths Inc. | Cerium oxides, zirconium oxides, Ce/Zr mixed oxides and Ce/Zr solid solutions having improved thermal stability and oxygen storage capacity |
FR2789601B1 (fr) * | 1999-02-17 | 2001-05-11 | Rhodia Chimie Sa | Sol organique et compose solide a base d'oxyde de cerium et d'un compose amphiphile et procedes de preparation |
ATE286954T1 (de) * | 2000-06-29 | 2005-01-15 | Neuftec Ltd | Ein brennstoffzusatz |
WO2002090260A1 (en) * | 2001-05-07 | 2002-11-14 | The Trustees Of Columbia University In The City Of New York | Apparatus and method for preparing cerium oxide nanoparticles |
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RU2252913C1 (ru) * | 2003-10-13 | 2005-05-27 | Институт Катализа Им. Г.К. Борескова Сибирского Отделения Российской Академии Наук | Способ получения синтез-газа |
WO2006046145A2 (en) * | 2004-10-25 | 2006-05-04 | Philip Morris Products S.A. | Gold-ceria catalyst for oxidation of carbon monoxide |
FR2884732B1 (fr) * | 2005-04-20 | 2007-08-24 | Rhodia Chimie Sa | Dispersion colloidale d'un compose de cerium et d'un autre element choisi parmi le zirconium, les terres rares, le titane et l'etain, solide dispersible a base de ce compose et procedes de preparation |
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CN102281945A (zh) | 2011-12-14 |
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EP2379221A1 (en) | 2011-10-26 |
AU2008365234A1 (en) | 2011-07-07 |
BRPI0823310B1 (pt) | 2018-02-14 |
KR101605465B1 (ko) | 2016-03-22 |
CA2747547C (en) | 2017-10-17 |
RU2487753C2 (ru) | 2013-07-20 |
CA2747547A1 (en) | 2010-06-24 |
BRPI0823310A8 (pt) | 2015-11-24 |
EP2379221A4 (en) | 2013-05-15 |
WO2010071641A1 (en) | 2010-06-24 |
JP2012512127A (ja) | 2012-05-31 |
AU2008365234B2 (en) | 2015-05-07 |
KR20110106884A (ko) | 2011-09-29 |
BRPI0823310A2 (pt) | 2015-06-23 |
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