JP6855073B2 - 多元系固溶体微粒子及びその製造方法並びに触媒 - Google Patents
多元系固溶体微粒子及びその製造方法並びに触媒 Download PDFInfo
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- JP6855073B2 JP6855073B2 JP2018503364A JP2018503364A JP6855073B2 JP 6855073 B2 JP6855073 B2 JP 6855073B2 JP 2018503364 A JP2018503364 A JP 2018503364A JP 2018503364 A JP2018503364 A JP 2018503364A JP 6855073 B2 JP6855073 B2 JP 6855073B2
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Images
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- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
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- B01D53/864—Removing carbon monoxide or hydrocarbons
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- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
- B01D53/86—Catalytic processes
- B01D53/8643—Removing mixtures of carbon monoxide or hydrocarbons and nitrogen oxides
- B01D53/8646—Simultaneous elimination of the components
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B01D53/34—Chemical or biological purification of waste gases
- B01D53/92—Chemical or biological purification of waste gases of engine exhaust gases
- B01D53/94—Chemical or biological purification of waste gases of engine exhaust gases by catalytic processes
- B01D53/944—Simultaneously removing carbon monoxide, hydrocarbons or carbon making use of oxidation catalysts
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01D53/34—Chemical or biological purification of waste gases
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Description
項1. 下記式:
PdxRuyMz(MはRh、Pt、Cu、Ag、Au及びIrからなる群から選ばれる少なくとも1種である。x+y+z=1、x+y=0.01〜0.99、z=0.99〜0.01、x:y=0.1:0.9〜0.9:0.1)
で表される多元系固溶体微粒子。
項2. MがRh、Pt、Cu、Ag、Au及びIrからなる群から選ばれる1種又は2種である、項1に記載の多元系固溶体微粒子。
項3. MがM1 pM2 q(式中、M1とM2は互いに異なって、Rh、Pt、Cu、Ag、Au及びIrからなる群から選ばれる。p=0.01〜0.99、q=0.99〜0.01、p+q=1)で表される、項1に記載の多元系固溶体微粒子。
項4. M1とM2が、IrとRhの組み合わせ、IrとPtの組み合わせ、RhとPtの組み合わせのいずれかである、項3に記載の多元系固溶体微粒子。
項5. MがRhである、項1に記載の多元系固溶体微粒子。
項6. x+y=0.05〜0.95、z=0.95〜0.05、x:y=0.15:0.85〜0.85:0.15である。項1に記載の多元系固溶体微粒子。
項7. x+y=0.1〜0.9、z=0.9〜0.1、x:y=0.2:0.8〜0.8:0.2である、項1に記載の多元系固溶体微粒子。
項8. 項1〜7のいずれか1項に記載の多元系固溶体微粒子を構成要素として含む触媒。
項9. 項8に記載の触媒を担体に担持してなる担持触媒。
項10. 担体が酸化物類を含む担体である、項9に記載の担持触媒。
項11. 排ガス浄化用触媒である、項9に記載の担持触媒。
項12. Rh塩、Pt塩、Cu塩、Ag塩、Au塩及びIr塩からなる群から選ばれる少なくとも1種とPd塩、Ru塩を含む水溶液を150℃〜250℃に加熱した液体還元剤に加えて反応させることを特徴とする、項1〜7のいずれか1項に記載の多元系固溶体微粒子の製造方法。
項13. Rh塩、Pt塩、Cu塩、Ag塩、Au塩及びIr塩からなる群から選ばれる少なくとも1種とPd塩、Ru塩を含む水溶液および担体を150℃〜250℃に加熱した液体還元剤に加えて反応させることを特徴とする、項9又は10に記載の担持触媒の製造方法。
項14. 担体が酸化物類を含む担体である、項13に記載の方法。
PdxRuyMz
(MはRh、Pt、Cu、Ag、Au及びIrからなる群から選ばれる少なくとも1種である。x+y+z=1、x+y=0.01〜0.99、z=0.99〜0.01、x:y=0.1:0.9〜0.9:0.1)で表される多元系固溶体微粒子である。PdとRuの合計のモル比率(x+y)は、多元系固溶体微粒子の好ましくは1〜99%、より好ましくは5〜95%、さらに好ましくは10〜90%であり、追加の金属(M)のモル比率(z)は、多元系固溶体微粒子の好ましくは99〜1%、より好ましくは95〜5%、さらに好ましくは90〜10%である。
Pd: K2PdCl4, Na2PdCl4, K2PdBr4, Na2PdBr4、硝酸パラジウムなど
Ru: RuCl3, RuBr3などのハロゲン化ルテニウム、硝酸ルテニウムなど
Rh: 酢酸ロジウム、硝酸ロジウム、塩化ロジウムなど
Pt: K2PtCl4、(NH4)2K2PtCl4、(NH4)2PtCl6、Na2PtCl6など
Au: 塩化金酸、臭化金酸、酢酸金など。
Ir:塩化イリジウム、イリジウムアセチルアセトナート、イリジウムシアン酸カリウム、イリジウム酸カリウムなど。
Ag:硝酸銀、酢酸銀など
Cu: 硫酸銅、塩化第1銅、塩化第2銅、酢酸銅、硝酸銅など。
トリエチレングリコール300mlを200℃で加熱撹拌し、この溶液にK2PdCl4(0.33mmol)とRuCl3(0.33mmol)と塩化ロジウム(0.33mmol)をイオン交換水40mlに溶かした溶液を加え、200℃で5分間維持した後放冷し、生じた沈殿物を遠心分離により分離した。分離した固溶状態のPd1/3Ru1/3Rh1/33元系固溶体微粒子について、XRDパターン(図1)及びそのピーク位置(表1)、TEM画像(図2)、STEM−EDX画像、HAADF−STEM画像(図3、図4)を測定した。
実施例1で得られた、乾燥後の合金微粒子を所定量秤量し、これを精製水に投入して超音波で処理することによって、合金微粒子の分散液を得た。このとき、秤量する合金微粒子の量は、元素分析によって予め求めた各金属の含有量を元に計算して決定した。この分散液に、800℃で5時間予備焼成したγ−アルミナの粉体(触媒学会参照触媒JRC−ALO8)を加え、マグネットスターラーを用いて12時間撹拌した。撹拌後の液をロータリーエバポレータに移し、減圧下で60℃に加熱し、粉体状になるまで乾燥させた。その後、得られた粉体から完全に水分を除去するため、120℃の乾燥機内に粉体を8時間静置した。乾燥後の粉体を乳鉢で充分に粉砕した後、一軸成形器によって1.2MPa、5分間の条件で円盤状に成形した。得られた成形物を破砕し、その後に篩にかけることによって、直径180〜250μmの粒状にした。このようにして、アルミナ粉末にPdRuRh3元系固溶体微粒子が1質量%担持された触媒を得た。得られた触媒について、1000℃×10h、燃料リッチ雰囲気条件で耐久性試験を行った。結果を図5に示す。
トリエチレングリコール300mlを200℃で加熱撹拌し、この溶液にK2PdCl4(0.5mmol)とRuCl3(0.5mmol)をイオン交換水40mlに溶かした溶液を加え、200℃で5分間維持した後放冷し、生じた沈殿物を遠心分離して固溶状態のPd0.5Ru0.52元系固溶体微粒子を分離した。
エチレングリコール200mlを196℃で加熱撹拌し、この溶液に塩化ロジウム(5.0mmol)をイオン交換水20mlに溶かした溶液を加え、90分間加熱攪拌した後、放冷し、生じた沈殿物を遠心分離してRh微粒子を分離した。
実施例2で得られたPd1/3Ru1/3Rh1/3合金微粒子を触媒として用いて、窒素酸化物(NOx)の還元反応、一酸化炭素(CO)の酸化反応に対する触媒活性および炭化水素(C3H6)の酸化反応に対する触媒活性を同時に評価した。また、比較のために、Pd0.5Ru0.5合金微粒子(比較例1)、Rh微粒子(比較例2)担持触媒も同様の方法で作製した。
トリエチレングリコール300ml、PVP(2mmol)、NaOH(10mmol)の混合物を225℃で加熱撹拌し、この溶液にK2PdCl4(0.2mmol)とRuCl3(0.2mmol)とCuSO4・5H2O(0.2mmol)をイオン交換水40mlに溶かした溶液を220℃をキープするようにスプレーし、スプレー後に220℃を10分間維持した後放冷し、生じた沈殿物を遠心分離により分離した。分離した固溶状態のPd1/3Ru1/3Cu1/33元系固溶体微粒子について、STEM-EDX画像及びHAADF-STEM画像(図10)、XRDパターン(図11)及びTEM画像(図12)を測定した。3元系固溶体微粒子の平均粒径は、2〜4nmであった。
実施例3において、CuSO4・5H2O(0.2mmol)に代えてIrCl4(0.2mmol)を使用する以外は実施例3と同様にしてPd1/3Ru1/3Ir1/33元系固溶体微粒子を製造した。得られたPd1/3Ru1/3Ir1/33元系固溶体微粒子について、STEM-EDX画像及びHAADF-STEM画像(図13)を測定した。
実施例3において、CuSO4・5H2O(0.2mmol)に代えてK2PtCl4(0.2mmol)を使用する以外は実施例3と同様にしてPd1/3Ru1/3Pt1/33元系固溶体微粒子を製造した。得られたPd1/3Ru1/3Pt1/33元系固溶体微粒子について、STEM-EDX画像及びHAADF-STEM画像(図14)を測定した。
実施例2で得られたPd1/3Ru1/3Rh1/3合金微粒子、実施例4で得られたPd1/3Ru1/3Ir1/3固溶体微粒子を600℃、800℃又は1000℃で10時間空気雰囲気で焼成し、Ruの残量を測定した。結果を図15に示す。Ruは高温酸化雰囲気下でRuO4として揮発してしまうが、PdRuIrとすることで、PdRuRhよりも更に高温までRuの耐久性が向上した。
トリエチレングリコール300ml、PVP(10mmol)の混合物を225℃で加熱撹拌し、この溶液にK2PdCl4(0.25mmol)、RuCl3(0.25mmol)、IrCl4(0.25mmol)、RhCl3(0.25mmol)をイオン交換水40mlに溶かした溶液を225℃をキープするようにスプレーし、スプレー後に225℃を10分間維持した後放冷し、生じた沈殿物を遠心分離により分離した。分離した固溶状態のPdRuIrRh4元系固溶体微粒子について、XRDパターン(図16a)、TEM画像(図16b)、線分析(図16c)、HAADF-STEM画像及びSTEM-EDX画像(図17)を測定した。
トリエチレングリコール300ml、PVP(10mmol)の混合物を225℃で加熱撹拌し、この溶液にK2PdCl4(0.25mmol)、RuCl3(0.25mmol)、K2PtCl4(0.25mmol)、IrCl4(0.25mmol)をイオン交換水40mlに溶かした溶液を225℃をキープするようにスプレーし、スプレー後に225℃を10分間維持した後放冷し、生じた沈殿物を遠心分離により分離した。分離した固溶状態のPdRuIrPt4元系固溶体微粒子について、XRDパターン(図18a)、TEM画像(図18b)、線分析(図18c)、HAADF-STEM画像及びSTEM-EDX画像(図19)を測定した。
トリエチレングリコール300ml、PVP(10mmol)の混合物を220℃で加熱撹拌し、この溶液にK2PdCl4(0.25mmol)、RuCl3(0.25mmol)、K2PtCl4(0.25mmol)、RhCl3(0.25mmol)をイオン交換水40mlに溶かした溶液を220℃をキープするようにスプレーし、スプレー後に220℃を10分間維持した後放冷し、生じた沈殿物を遠心分離により分離した。分離した固溶状態のPdRuPtRh4元系固溶体微粒子について、XRDパターン(図20a)、TEM画像(図20b)、線分析(図20c)、HAADF-STEM画像及びSTEM-EDX画像(図21)を測定した。
トリエチレングリコール100ml、PVP(0.6mmol)の混合物を210℃で加熱撹拌し、この溶液にPdNO3(0.2mmol)とRu(COOCH3)3(0.2mmol)とAgNO3(0.2mmol)をイオン交換水10mlに溶かした溶液を210℃をキープするように1.0ml/minでシリンジポンプにより滴下し、滴下後に210℃を10分間維持した後放冷し、生じた沈殿物を遠心分離により分離した。分離した固溶状態のPd1/3Ru1/3Ag1/33元系固溶体微粒子について、STEM-EDX画像及びHAADF-STEM画像(図22)、XRDパターン(図23)及びTEM画像(図24)を測定した。3元系固溶体微粒子の平均粒径は、3.6±1.0nmであった。
トリエチレングリコール150ml、PVP(1mmol)の混合物を225℃で加熱撹拌し、この溶液にK2PdCl4(0.1mmol)とRuCl3(0.1mmol)とHAuCl4(0.1mmol)をイオン交換水20mlに溶かした溶液を225℃をキープするようにスプレーし、スプレー後に225℃を10分間維持した後放冷し、生じた沈殿物を遠心分離により分離した。分離した固溶状態のPd1/3Ru1/3Au1/33元系固溶体微粒子について、STEM-EDX画像及びHAADF-STEM画像(図25)、XRDパターン(図26)及びTEM画像(図27)を測定した。3元系固溶体微粒子の平均粒径は、5.8±1.9nmであった。
Claims (14)
- 下記式:
PdxRuyMz(MはRh、Pt、Cu及びIrからなる群から選ばれる少なくとも1種である。x+y+z=1、x+y=0.01〜0.99、z=0.99〜0.01、x:y=0.1:0.9〜0.9:0.1)
で表される多元系固溶体微粒子。 - MがRh、Pt、Cu及びIrからなる群から選ばれる1種又は2種である、請求項1に記載の多元系固溶体微粒子。
- MがM1 pM2 q(式中、M1とM2は互いに異なって、Rh、Pt、Cu及びIrからなる群から選ばれる。p=0.01〜0.99、q=0.99〜0.01、p+q=1)で表される、請求項1に記載の多元系固溶体微粒子。
- M1とM2が、IrとRhの組み合わせ、IrとPtの組み合わせ、RhとPtの組み合わせのいずれかである、請求項1に記載の多元系固溶体微粒子。
- MがRhである、請求項1に記載の多元系固溶体微粒子。
- x+y=0.05〜0.95、z=0.95〜0.05、x:y=0.15:0.85〜0.85:0.15である。請求項1に記載の多元系固溶体微粒子。
- x+y=0.1〜0.9、z=0.9〜0.1、x:y=0.2:0.8〜0.8:0.2である、請求項1に記載の多元系固溶体微粒子。
- 請求項1〜7のいずれか1項に記載の多元系固溶体微粒子を構成要素として含む触媒。
- 請求項8に記載の触媒を担体に担持してなる担持触媒。
- 担体が酸化物類を含む担体である、請求項9に記載の担持触媒。
- 排ガス浄化用触媒である、請求項9に記載の担持触媒。
- Rh塩、Pt塩、Cu塩及びIr塩からなる群から選ばれる少なくとも1種とPd塩、Ru塩を含む水溶液を150℃〜250℃に加熱した液体還元剤に加えて反応させることを特徴とする、請求項1〜7のいずれか1項に記載の多元系固溶体微粒子の製造方法。
- Rh塩、Pt塩、Cu塩及びIr塩からなる群から選ばれる少なくとも1種とPd塩、Ru塩を含む水溶液および担体を150℃〜250℃に加熱した液体還元剤に加えて反応させることを特徴とする、請求項9又は10に記載の担持触媒の製造方法。
- 担体が酸化物類を含む担体である、請求項13に記載の方法。
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