JP2006297234A - 複合体の製法 - Google Patents
複合体の製法 Download PDFInfo
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- JP2006297234A JP2006297234A JP2005120333A JP2005120333A JP2006297234A JP 2006297234 A JP2006297234 A JP 2006297234A JP 2005120333 A JP2005120333 A JP 2005120333A JP 2005120333 A JP2005120333 A JP 2005120333A JP 2006297234 A JP2006297234 A JP 2006297234A
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- 239000002131 composite material Substances 0.000 title claims abstract description 26
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 24
- 239000002245 particle Substances 0.000 claims abstract description 79
- 239000002243 precursor Substances 0.000 claims abstract description 75
- 239000010419 fine particle Substances 0.000 claims abstract description 71
- 238000000034 method Methods 0.000 claims abstract description 25
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- 238000003786 synthesis reaction Methods 0.000 claims abstract description 12
- CYIDZMCFTVVTJO-UHFFFAOYSA-N pyromellitic acid Chemical compound OC(=O)C1=CC(C(O)=O)=C(C(O)=O)C=C1C(O)=O CYIDZMCFTVVTJO-UHFFFAOYSA-N 0.000 claims description 16
- 239000011232 storage material Substances 0.000 claims description 12
- IWOUKMZUPDVPGQ-UHFFFAOYSA-N barium nitrate Chemical compound [Ba+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O IWOUKMZUPDVPGQ-UHFFFAOYSA-N 0.000 claims description 6
- XNGIFLGASWRNHJ-UHFFFAOYSA-N phthalic acid Chemical compound OC(=O)C1=CC=CC=C1C(O)=O XNGIFLGASWRNHJ-UHFFFAOYSA-N 0.000 claims description 6
- 229910052783 alkali metal Inorganic materials 0.000 claims description 5
- 150000001340 alkali metals Chemical class 0.000 claims description 5
- 229910052784 alkaline earth metal Inorganic materials 0.000 claims description 5
- 150000001342 alkaline earth metals Chemical class 0.000 claims description 5
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- OFOBLEOULBTSOW-UHFFFAOYSA-N Propanedioic acid Natural products OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 claims description 3
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- VZCYOOQTPOCHFL-UPHRSURJSA-N maleic acid Chemical compound OC(=O)\C=C/C(O)=O VZCYOOQTPOCHFL-UPHRSURJSA-N 0.000 claims description 3
- 239000011976 maleic acid Substances 0.000 claims description 3
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 claims description 3
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- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 2
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 2
- 230000002194 synthesizing effect Effects 0.000 abstract description 4
- 239000003054 catalyst Substances 0.000 description 33
- 239000000243 solution Substances 0.000 description 21
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 14
- 231100000572 poisoning Toxicity 0.000 description 14
- 230000000607 poisoning effect Effects 0.000 description 14
- AYJRCSIUFZENHW-UHFFFAOYSA-L barium carbonate Chemical compound [Ba+2].[O-]C([O-])=O AYJRCSIUFZENHW-UHFFFAOYSA-L 0.000 description 12
- 238000000746 purification Methods 0.000 description 12
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 11
- 239000000463 material Substances 0.000 description 11
- 229910052717 sulfur Inorganic materials 0.000 description 11
- 239000011593 sulfur Substances 0.000 description 11
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 10
- 239000007789 gas Substances 0.000 description 10
- 150000003839 salts Chemical class 0.000 description 10
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 9
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- 239000010948 rhodium Substances 0.000 description 5
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- 229910052703 rhodium Inorganic materials 0.000 description 4
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- ITHZDDVSAWDQPZ-UHFFFAOYSA-L barium acetate Chemical compound [Ba+2].CC([O-])=O.CC([O-])=O ITHZDDVSAWDQPZ-UHFFFAOYSA-L 0.000 description 3
- 238000002485 combustion reaction Methods 0.000 description 3
- 229910052746 lanthanum Inorganic materials 0.000 description 3
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 description 3
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- 229910052788 barium Inorganic materials 0.000 description 2
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 description 2
- 239000002585 base Substances 0.000 description 2
- 229910002091 carbon monoxide Inorganic materials 0.000 description 2
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- 239000002184 metal Substances 0.000 description 2
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- 239000000758 substrate Substances 0.000 description 2
- 239000011882 ultra-fine particle Substances 0.000 description 2
- RUDFQVOCFDJEEF-UHFFFAOYSA-N yttrium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Y+3].[Y+3] RUDFQVOCFDJEEF-UHFFFAOYSA-N 0.000 description 2
- 239000001763 2-hydroxyethyl(trimethyl)azanium Substances 0.000 description 1
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 description 1
- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 description 1
- 235000019743 Choline chloride Nutrition 0.000 description 1
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- 239000013543 active substance Substances 0.000 description 1
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- 235000012538 ammonium bicarbonate Nutrition 0.000 description 1
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- AYJRCSIUFZENHW-DEQYMQKBSA-L barium(2+);oxomethanediolate Chemical compound [Ba+2].[O-][14C]([O-])=O AYJRCSIUFZENHW-DEQYMQKBSA-L 0.000 description 1
- 229960000686 benzalkonium chloride Drugs 0.000 description 1
- CADWTSSKOVRVJC-UHFFFAOYSA-N benzyl(dimethyl)azanium;chloride Chemical compound [Cl-].C[NH+](C)CC1=CC=CC=C1 CADWTSSKOVRVJC-UHFFFAOYSA-N 0.000 description 1
- 150000004649 carbonic acid derivatives Chemical class 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- RCFVMJKOEJFGTM-UHFFFAOYSA-N cerium zirconium Chemical compound [Zr].[Ce] RCFVMJKOEJFGTM-UHFFFAOYSA-N 0.000 description 1
- SGMZJAMFUVOLNK-UHFFFAOYSA-M choline chloride Chemical compound [Cl-].C[N+](C)(C)CCO SGMZJAMFUVOLNK-UHFFFAOYSA-M 0.000 description 1
- 229960003178 choline chloride Drugs 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
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Abstract
【解決手段】 担体粒子に、該担体粒子より小径の被担持微粒子を吸着かつ担持させてなる複合体の製法において、前記担体粒子もしくはその前駆体を、これに吸着させるべき前記被担持微粒子もしくはその前駆体とは逆の電位に帯電させる第1の工程と、難溶性の前記被担持微粒子もしくはその前駆体を合成するとともにその合成の直後もしくは合成液中で前記難溶性の前記被担持微粒子もしくはその前駆体を前記担体粒子もしくはその前駆体に吸着させる第2の工程とを有することを特徴とする方法。
【選択図】 図2
Description
操作手順は、図2のフローチャートに示すとおりであり、従来知られている適宜の方法によって、アルミナとチタニアとジルコニアとの混合物からなる担体を、予めモノリス基材にコートし、これに白金およびロジウムなどの貴金属を担持した触媒を用意する。その触媒を、ピロメリト酸飽和溶液中に浸漬して、ピロメリト酸を吸着する。つぎに、0.4モルの酢酸バリウムを約4リットルの蒸留水に溶解した液に、炭酸水素アンモニウムの1モル溶液を300ml(ミリリットル)加えて撹拌した。このときpHは6.5に低下して、炭酸バリウム微粒子が生成した。
上記の触媒をピロメリト酸液から取り出すとともに過剰に付着しているピロメリト酸を吹き払い、これを、上記の炭酸バリウムを生成させた液に、従来知られている貴金属の含浸の場合と同様にして浸漬することにより、炭酸バリウム微粒子を触媒に吸着させた。この吸着にはおおよそ30分を要した。
得られた触媒組成は、Pt:2g/L(触媒の1リットル)、Rh:0.5g/L、Ba/K=0.2/1mol/L、担体:アルミナ、チタニア、ジルコニアの混合物。
図3のフローチャートに概略を示すように吸水担持法によって担持させた。先ず、従来知られている適宜の触媒担体を用意する。また一方、高濃度のアルカリ土類イオン溶液を作る。この溶液を上記の担体の細孔に吸収させた後、過剰に付着している溶液を吹き払い、乾燥をおこなった後に焼成することにより、アルカリ土類の塩を上記の担体上に担持させる。
酢酸バリウムを用いた場合の例として、5.17gの酢酸バリウムを、4リットルの蒸留水に溶解した後、その溶液に、既存の方法でモノリス基材2リットルにアルミナおよびチタニアならびにジルコニアからなる触媒担体をコートし、白金およびロジウムなどの貴金属を担持した触媒を浸漬して、その触媒の細孔内に上記の溶液を満たす。直ちに触媒を溶液から引き上げ、過剰に付着している溶液を吹き払った後、120℃の温風で乾燥した。得られた触媒組成は、上記の実施例と同様である。
実施例で得られた触媒と比較例で得られた触媒についてSOX(ソックス)による被毒および被毒からの再生の評価をおこなった。内燃機関の排ガスとして希薄燃焼(リーン)時の排ガスと、ストイキもしくはそれより空燃比の小さいリッチ時の排ガスとを流した。空間速度SV=50000h-1、リーン運転を1分継続し、その後にリッチ運転を30秒おこなう運転を所定時間継続した。リーン運転時の排ガスの組成は、NOx:250ppm、O2:6%、H2O:8%、CO2:10%である。リッチ運転時の排ガスの組成は、O2:0%、CO:6000ppm、その他はリーン運転と同じである。
イオウ被毒条件は、温度を250〜550℃、通過イオウ量を触媒1リットルに対して6g(6g/L)とした。また、イオウ再生条件は、温度を650℃、空燃比(A/F)が“14”相当の排ガスを10分間、流通させた。得られた結果は、表1のとおりである。
これに対して比較例による触媒では、ソックス被毒再生繰り返し後のNOx浄化率が低下することが認められ、その傾向は温度が高いほど顕著になり、550℃では1/8程度に低下し、イオウ被毒し易く、またその再生が困難であることが認められた。これは、NOx吸蔵材である被担持微粒子が大径化していることによるものと思われる。
Claims (7)
- 担体粒子に、該担体粒子より小径の被担持微粒子を吸着かつ担持させてなる複合体の製法において、
前記担体粒子もしくはその前駆体を、これに吸着させるべき前記被担持微粒子もしくはその前駆体とは逆の電位に帯電させる第1の工程と、難溶性の前記被担持微粒子もしくはその前駆体を合成するとともにその合成の直後もしくは合成液中で前記難溶性の前記被担持微粒子もしくはその前駆体を前記担体粒子もしくはその前駆体に吸着させる第2の工程とを有することを特徴とする複合体の製法。 - 前記担体粒子が複合酸化物からなり、かつ前記被担持微粒子がNOx吸蔵材からなることを特徴とする請求項1に記載の複合体の製法。
- 前記NOx吸蔵材の粒子成分が、アルカリ金属もしくはアルカリ土類金属の一種以上の元素成分であり、その難溶性の微粒子もしくはその前駆体が炭酸塩、シュウ酸塩、硫酸塩のいずれかあるいは硝酸バリウムであることを特徴とする請求項2に記載の複合体の製法。
- 前記第1の工程では、前記被担持微粒子もしくはその前駆体の表面電位がプラスであって、前記担体粒子もしくはその前駆体の表面電位をマイナスに帯電させることを特徴とする請求項1から3のいずれかに記載の複合体の製法。
- 前記被担持微粒子もしくはその前駆体を前記担体粒子もしくはその前駆体に吸着させる雰囲気のpHを、前記難溶性の微粒子もしくはその前駆体の表面電位が+5〜+40mVとなるpHに設定することを特徴とする請求項3または4に記載の複合体の製法。
- 前記担体粒子もしくはその前駆体を、これに吸着させるべき前記被担持微粒子もしくはその前駆体とは逆の電位に帯電させる第1の工程が、前記担体粒子もしくはその前駆体の表面に有機酸を予め吸着させる工程であることを特徴とする請求項1から5のいずれかに記載の複合体の製法。
- 前記有機酸が、ピロメリト酸、マレイン酸、フタル酸のいずれかであることを特徴とする請求項6に記載の複合体の製法。
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CN101918135A (zh) * | 2009-03-18 | 2010-12-15 | 丰田自动车株式会社 | 纳米粒子的担载方法 |
WO2024018268A1 (en) * | 2022-07-19 | 2024-01-25 | Universidade De Coimbra | Core-shell alumina-silica nanoparticles, method of producing the same and composite construction materials comprising the nanoparticles for fire protection |
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