JP5827567B2 - 触媒担体又は触媒の製造方法 - Google Patents
触媒担体又は触媒の製造方法 Download PDFInfo
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- 239000003054 catalyst Substances 0.000 title claims description 110
- 238000004519 manufacturing process Methods 0.000 title claims description 22
- 239000007864 aqueous solution Substances 0.000 claims description 92
- 239000011148 porous material Substances 0.000 claims description 71
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 56
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 claims description 52
- 238000000746 purification Methods 0.000 claims description 51
- 239000011777 magnesium Substances 0.000 claims description 48
- 238000011049 filling Methods 0.000 claims description 43
- 229910000510 noble metal Inorganic materials 0.000 claims description 43
- 229910052749 magnesium Inorganic materials 0.000 claims description 40
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 claims description 33
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 claims description 33
- -1 magnesium aluminate Chemical class 0.000 claims description 32
- UAMZXLIURMNTHD-UHFFFAOYSA-N dialuminum;magnesium;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[Mg+2].[Al+3].[Al+3] UAMZXLIURMNTHD-UHFFFAOYSA-N 0.000 claims description 29
- 238000002360 preparation method Methods 0.000 claims description 29
- 238000000034 method Methods 0.000 claims description 27
- 238000001035 drying Methods 0.000 claims description 23
- 229910052763 palladium Inorganic materials 0.000 claims description 23
- 238000010304 firing Methods 0.000 claims description 19
- 238000002485 combustion reaction Methods 0.000 claims description 11
- 229910001425 magnesium ion Inorganic materials 0.000 claims description 6
- JLVVSXFLKOJNIY-UHFFFAOYSA-N Magnesium ion Chemical compound [Mg+2] JLVVSXFLKOJNIY-UHFFFAOYSA-N 0.000 claims description 5
- 239000002344 surface layer Substances 0.000 claims description 5
- 230000009471 action Effects 0.000 claims description 4
- 229930195733 hydrocarbon Natural products 0.000 description 29
- 150000002430 hydrocarbons Chemical class 0.000 description 29
- 239000004215 Carbon black (E152) Substances 0.000 description 28
- 230000000694 effects Effects 0.000 description 26
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 23
- 229910002091 carbon monoxide Inorganic materials 0.000 description 23
- 239000007789 gas Substances 0.000 description 23
- 229910052596 spinel Inorganic materials 0.000 description 22
- 239000011029 spinel Substances 0.000 description 22
- 230000000052 comparative effect Effects 0.000 description 18
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 15
- 239000001301 oxygen Substances 0.000 description 14
- 229910052760 oxygen Inorganic materials 0.000 description 14
- 238000001354 calcination Methods 0.000 description 13
- 238000002474 experimental method Methods 0.000 description 13
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 8
- 238000011156 evaluation Methods 0.000 description 7
- 239000010419 fine particle Substances 0.000 description 7
- 238000010438 heat treatment Methods 0.000 description 7
- 239000000843 powder Substances 0.000 description 7
- YIXJRHPUWRPCBB-UHFFFAOYSA-N magnesium nitrate Chemical compound [Mg+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O YIXJRHPUWRPCBB-UHFFFAOYSA-N 0.000 description 6
- 239000000203 mixture Substances 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- ATUOYWHBWRKTHZ-UHFFFAOYSA-N Propane Chemical compound CCC ATUOYWHBWRKTHZ-UHFFFAOYSA-N 0.000 description 4
- 239000000446 fuel Substances 0.000 description 4
- 150000002500 ions Chemical class 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 3
- MWUXSHHQAYIFBG-UHFFFAOYSA-N Nitric oxide Chemical compound O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 3
- 230000003197 catalytic effect Effects 0.000 description 3
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 3
- 239000000395 magnesium oxide Substances 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 3
- 238000006722 reduction reaction Methods 0.000 description 3
- 229910017771 LaFeO Inorganic materials 0.000 description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 2
- 230000002378 acidificating effect Effects 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 2
- 150000001342 alkaline earth metals Chemical class 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 229910000420 cerium oxide Inorganic materials 0.000 description 2
- HSJPMRKMPBAUAU-UHFFFAOYSA-N cerium(3+);trinitrate Chemical compound [Ce+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O HSJPMRKMPBAUAU-UHFFFAOYSA-N 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 239000012153 distilled water Substances 0.000 description 2
- 239000010410 layer Substances 0.000 description 2
- MFUVDXOKPBAHMC-UHFFFAOYSA-N magnesium;dinitrate;hexahydrate Chemical compound O.O.O.O.O.O.[Mg+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MFUVDXOKPBAHMC-UHFFFAOYSA-N 0.000 description 2
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 2
- 239000011572 manganese Substances 0.000 description 2
- 239000004570 mortar (masonry) Substances 0.000 description 2
- 229910017604 nitric acid Inorganic materials 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 description 2
- 239000001294 propane Substances 0.000 description 2
- 239000010948 rhodium Substances 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 229910052684 Cerium Inorganic materials 0.000 description 1
- 238000004566 IR spectroscopy Methods 0.000 description 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 1
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 1
- 229910002651 NO3 Inorganic materials 0.000 description 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
- 230000010718 Oxidation Activity Effects 0.000 description 1
- 230000010757 Reduction Activity Effects 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 150000001340 alkali metals Chemical class 0.000 description 1
- 150000004645 aluminates Chemical class 0.000 description 1
- SNAAJJQQZSMGQD-UHFFFAOYSA-N aluminum magnesium Chemical compound [Mg].[Al] SNAAJJQQZSMGQD-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 229910052788 barium Inorganic materials 0.000 description 1
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 description 1
- 229910001422 barium ion Inorganic materials 0.000 description 1
- 229910052728 basic metal Inorganic materials 0.000 description 1
- 150000003818 basic metals Chemical class 0.000 description 1
- 150000004649 carbonic acid derivatives Chemical class 0.000 description 1
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 238000012790 confirmation Methods 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000000295 fuel oil Substances 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 229910052746 lanthanum Inorganic materials 0.000 description 1
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 150000002823 nitrates Chemical class 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 1
- 150000002940 palladium Chemical class 0.000 description 1
- GPNDARIEYHPYAY-UHFFFAOYSA-N palladium(ii) nitrate Chemical compound [Pd+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O GPNDARIEYHPYAY-UHFFFAOYSA-N 0.000 description 1
- 239000008188 pellet Substances 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 239000010970 precious metal Substances 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 229910052703 rhodium Inorganic materials 0.000 description 1
- MHOVAHRLVXNVSD-UHFFFAOYSA-N rhodium atom Chemical compound [Rh] MHOVAHRLVXNVSD-UHFFFAOYSA-N 0.000 description 1
- 238000007873 sieving Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 229910001928 zirconium oxide Inorganic materials 0.000 description 1
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Description
即ち、ペロブスカイト型複合酸化物触媒を用いた従来のものは、900℃で100時間の熱処理をしたあとでもHCやCO、NO浄化性能に劣化がなく、すでに実車に搭載されるに至っている。しかし、近時においては、燃焼装置の熱効率改善の観点からより高温での燃焼技術が開発されており、それに伴って燃焼排ガスの温度も上昇していることから、冷間時排ガス浄化のため、エンジン直下に設置される触媒は900℃を超える高温環境下となることもあり、上記従来の触媒では当該高性能燃焼装置に適用した場合、耐熱性及び耐久性に十分ではないという問題があった。
本実施形態に係る触媒担体は、80〜150(m2/g)の範囲の比表面積、及び0.45〜0.65(ml/g)の範囲の細孔容積を有するマグネシウムアルミネート(MgAl2O4)から成り、その上に貴金属が担持可能とされたものであり、図1に示すように、水溶液調製工程S1と、水溶液充填工程S2と、乾燥工程S3と、仮焼工程S4及び焼成工程S5とを経て製造され、更には貴金属担持工程S6を経ることにより排ガス浄化触媒を得ることができる。
(実験1):マグネシウムアルミネート(MgAl2O4:スピネル)の合成及び特性化
MgOの前躯体として硝酸マグネシウム6水和物(Mg(NO3)2・6H2O)を用い、その25.6(g)(0.1(mol))を蒸留水に溶解させて10.2(ml)の硝酸マグネシウム水溶液を得た(水溶液調製工程)。この水溶液を10.2(g)(0.1(mol))の市販アルミナ粉末(比表面積:247(m2/g)、細孔容積:1.0(ml/g))に滴下し、乳鉢中で混合しながらその細孔内に当該水溶液を充填させた(ポアフィリング法による水溶液充填工程)。
8.3(wt%)のPd(パラジウム)を含むジニトロジアミンPdの硝酸酸性水溶液1.8(g)を、容積が2.4(ml)となるように蒸留水で希釈して水溶液を得た。この水溶液を、実験1で得られた実施例3の粉末5(g)に滴下し、乳鉢中で混合しながらその細孔内に当該水溶液を充填させた。
実験3で得られた実施例7をペレット状に成形した後、粉砕し、0.25〜1.0(mm)の粉末を篩分した。その0.5(ml)(約0.26(g)に相当)を用いて浄化活性を評価した。この活性評価に用いた模擬ガスの組成は、NO:1500(ppm)、CO:0.65(%)、C3H8:180(ppm)、C3H6:180(ppm)、O2:0.50(%)であり、バランスガスとして窒素を用いた。尚、ガス流量は、1(l/min)(空間速度:120000(hr−1)に相当)に設定した。
実験3と同様の方法にて、実施例8〜10に係る触媒及び比較例に係る触媒についても触媒活性を観察し、450(℃)及び500(℃)におけるHCやCO、NOの浄化率を測定した。また、実験3と同様、900(℃)で10時間、50時間、100時間、150時間、200時間(但し、比較例については150時間まで)熱処理した後、上記と同様の方法で450(℃)及び500(℃)におけるHCやCO、NOの浄化活性を測定した。測定結果について以下の表3〜6にまとめた。
通常、排気ガス中の酸素濃度は燃料の燃焼条件に応じて変化する。酸素濃度の大きい排気ガスは「リーン」、酸素濃度の小さい排気ガスは「リッチ」と呼ばれ、それぞれの条件により触媒の浄化性能も変化する。実験3で用いた模擬排ガス組成は、理論空燃比(燃焼に用いる空気と燃料の重量比が14.7)における燃焼排ガスとして、典型的な組成である。
S2 水溶液充填工程
S3 乾燥工程
S4 仮焼工程
S5 焼成工程
S6 貴金属担持工程
Claims (6)
- 多孔質アルミナの細孔内にマグネシウムアルミネート(MgAl2O4)を形成して成り、その上に貴金属が担持される燃焼装置の排ガス浄化用の触媒担体の製造方法であって、
マグネシウムイオンを含む水溶液を調製する水溶液調製工程と、
前記多孔質アルミナの細孔にて生じる毛細管現象を利用したポアフィリング法により当該細孔内に前記水溶液調製工程で得られた水溶液を充填する水溶液充填工程と、
該水溶液充填工程にて細孔内に水溶液が充填された多孔質アルミナを乾燥する乾燥工程と、
該乾燥工程で得られた多孔質アルミナを1000℃で焼成することにより、マグネシウムアルミネートを生成させる焼成工程と、
を含むとともに、前記水溶液調製工程で得られる水溶液の濃度を任意調整することにより、多孔質アルミナの表層をマグネシウムアルミネートとしつつ中心部のアルミナの状態を維持させることを特徴とする触媒担体の製造方法。 - 前記水溶液調製工程で得られる水溶液は、その濃度が任意調整されることにより、前記焼成工程にて前記多孔質アルミナに形成されるマグネシウムアルミネートの量を調整可能とされたことを特徴とする請求項1記載の触媒担体の製造方法。
- 前記焼成工程で生成されたマグネシウムアルミネートに二酸化セリウム(CeO2)を添加させる二酸化セリウム添加工程を有したことを特徴とする請求項1又は請求項2記載の触媒担体の製造方法。
- 多孔質アルミナの細孔内にマグネシウムアルミネート(MgAl2O4)を形成して成り、その上に貴金属を担持して成る燃焼装置の排ガス浄化用の触媒の製造方法であって、
マグネシウムイオンを含む水溶液を調製する水溶液調製工程と、
前記多孔質アルミナの細孔にて生じる毛細管現象を利用したポアフィリング法により当該細孔内に前記水溶液調製工程で得られた水溶液を充填する水溶液充填工程と、
該水溶液充填工程にて細孔内に水溶液が充填された多孔質アルミナを乾燥する乾燥工程と、
該乾燥工程で得られた多孔質アルミナを1000℃で焼成することにより、マグネシウムアルミネートを生成させる焼成工程と、
を有し、前記焼成工程で焼成された多孔質アルミナの細孔に対し、当該細孔にて生じる毛細管現象を利用したポアフィリング法により貴金属を含有した水溶液を充填するとともに、前記水溶液調製工程で得られる水溶液の濃度を任意調整することにより、多孔質アルミナの表層をマグネシウムアルミネートとしつつ中心部のアルミナの状態を維持させることを特徴とする触媒の製造方法。 - 前記貴金属がパラジウムであることを特徴とする請求項4記載の触媒の製造方法。
- 前記焼成工程で生成されたマグネシウムアルミネートに二酸化セリウム(CeO2)を添加させる二酸化セリウム添加工程を有し、当該二酸化セリウム添加工程を経た触媒担体に前記貴金属を担持させたことを特徴とする請求項4又は請求項5記載の触媒の製造方法。
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