JP6225400B2 - 外殻構造を有する触媒担持体用フェライト粒子 - Google Patents
外殻構造を有する触媒担持体用フェライト粒子 Download PDFInfo
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- JP6225400B2 JP6225400B2 JP2015013794A JP2015013794A JP6225400B2 JP 6225400 B2 JP6225400 B2 JP 6225400B2 JP 2015013794 A JP2015013794 A JP 2015013794A JP 2015013794 A JP2015013794 A JP 2015013794A JP 6225400 B2 JP6225400 B2 JP 6225400B2
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- particles
- ferrite
- ferrite particles
- outer shell
- shell structure
- Prior art date
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- 239000002245 particle Substances 0.000 title claims description 288
- 229910000859 α-Fe Inorganic materials 0.000 title claims description 209
- 239000003054 catalyst Substances 0.000 title claims description 46
- 239000010936 titanium Substances 0.000 claims description 37
- 239000011148 porous material Substances 0.000 claims description 36
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 8
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 claims description 8
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 8
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 5
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 4
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 claims description 4
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 4
- 229910017052 cobalt Inorganic materials 0.000 claims description 4
- 239000010941 cobalt Substances 0.000 claims description 4
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 4
- 229910052802 copper Inorganic materials 0.000 claims description 4
- 239000010949 copper Substances 0.000 claims description 4
- 229910052737 gold Inorganic materials 0.000 claims description 4
- 239000010931 gold Substances 0.000 claims description 4
- 229910052759 nickel Inorganic materials 0.000 claims description 4
- 229910052763 palladium Inorganic materials 0.000 claims description 4
- 229910052697 platinum Inorganic materials 0.000 claims description 4
- 229910052703 rhodium Inorganic materials 0.000 claims description 4
- 239000010948 rhodium Substances 0.000 claims description 4
- MHOVAHRLVXNVSD-UHFFFAOYSA-N rhodium atom Chemical compound [Rh] MHOVAHRLVXNVSD-UHFFFAOYSA-N 0.000 claims description 4
- 229910052707 ruthenium Inorganic materials 0.000 claims description 4
- 229910052751 metal Inorganic materials 0.000 claims description 3
- 239000002184 metal Substances 0.000 claims description 3
- 229910052709 silver Inorganic materials 0.000 claims description 3
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- 239000011248 coating agent Substances 0.000 description 40
- 238000000576 coating method Methods 0.000 description 40
- 238000010304 firing Methods 0.000 description 27
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- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 6
- 239000001301 oxygen Substances 0.000 description 6
- 229910052760 oxygen Inorganic materials 0.000 description 6
- 239000011258 core-shell material Substances 0.000 description 5
- 229910052749 magnesium Inorganic materials 0.000 description 5
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 5
- 229910052753 mercury Inorganic materials 0.000 description 5
- 238000002156 mixing Methods 0.000 description 5
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- 229910052719 titanium Inorganic materials 0.000 description 5
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
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- SZVJSHCCFOBDDC-UHFFFAOYSA-N iron(II,III) oxide Inorganic materials O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 description 2
- 229910052746 lanthanum Inorganic materials 0.000 description 2
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 description 2
- 229910052748 manganese Inorganic materials 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- 239000006104 solid solution Substances 0.000 description 2
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- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
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- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 1
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- 229910017604 nitric acid Inorganic materials 0.000 description 1
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Description
さらに、特許文献2(特開2004−189513号公報)には、フェライト粒子の表面にガラス質粒子を付着させ、溶融したガラス質層の被覆を形成させ、ガラス被覆フェライト粒子の表面に酸化チタンを被覆させ、再度熱処理する機能性フェライト粒子の製造方法が記載されており、この機能性フェライト粒子は光触媒材料として有用であるとされている。ここで用いられるフェライト粒子としては、MnZn系、MgCuZn系、NiCuZn系等が挙げられている。
Tiが固溶されたフェライトを含む外殻構造を有し、当該フェライト粒子内部に存在する細孔と当該外殻構造に存在する細孔とが連通し、当該フェライト粒子内部に存在する細孔及び当該外殻構造に存在する細孔は、細孔容積が0.06〜0.2ml/gであり、ピーク細孔径は0.7〜2μmであることを特徴とする触媒担持体用フェライト粒子を提供するものである。
<本発明に係るフェライト粒子>
本発明に係るフェライト粒子は、チタンを含有する外殻構造(コアシェル形状)を有する。このことで低い見掛け密度を有し、さまざまな特性を制御可能な状態に維持できる。また、本発明に係るフェライト粒子は、一定容積に少ない重量でフェライト粒子を満たすことができる。なお、本発明でいうフェライト粒子とは、特記しない限り個々のフェライト粒子の集合体を意味し、また単に粒子とは、個々のフェライト粒子をいう。
ここで、粒子の外殻構造の厚さの測定は下記の手順にて行う。
フェライト粒子を樹脂に包埋・成形したのち、研磨機にて断面を研磨し、金蒸着を行い断面観察用(外殻部の厚さ測定用)サンプルとした。得られたサンプルは日本電子社製JSM−6060Aを用い、加速電圧は5kVとし、SEMを200倍視野にて撮影し、その画像情報を、インターフェースを介してメディアサイバネティクス社製画像解析ソフト(Image−Pro PLUS)に導入して解析を行った。具体的には得られた画像のコントラストを調整後、本解析ソフトウエアのラインプロファイル機能により、画像の輝度を1粒子ごとに抽出する。この時ラインプロファイルは粒子のほぼ中心を水平方向に通過するよう直線を設定し、得られたプロファイルに存在するピークのうち、外殻部に対応するピークを2つのマーカーで挟み、このときの幅を外殻部の厚さとした。なお、上記ピークはラインプロファイルの極大値を挟む極小値と極小値として定義される。また、コントラストは包埋樹脂の部分(バックグラウンドに相当)の輝度は最大輝度の50%以下になるように調整することが好ましい。同様の操作を30粒子について同様に行い、平均値を外殻構造の厚さとした。
上記と同様の画像処理を行い、ラインプロファイルを円環または自由曲線(閉曲線)とし1粒子ごとに粒子の外殻構造に対して設定する。このときプロファイルの最大輝度をI最大、最小輝度をI最小とし、最大輝度と最小輝度の差をIΔとしたとき、I最小以上、I最小+IΔ×0.2未満の範囲は外殻構造がない部分、I最小+IΔ×0.2以上I最大 以下が外殻部と判別する。したがってラインプロファイル機能で得られたラインプロファイル長(周囲長)の輝度データのうち、I最小+IΔ×0.2以上I最大以下となっている輝度のラインプロファイル長を積算し、ラインプロファイル長(周囲長)で割ることで、一定範囲の厚みを持った外周部分の比率を算出することで求めることができる。同様の操作を30粒子について行い、平均値を外周部分の周囲長にしめる割合(=外周部分の密度)とした。
これらFe、Mg、Ti及びSrの含有量は、下記によって測定される。
フェライト粒子(フェライトキャリア芯材)0.2gを秤量し、純水60mlに1Nの塩酸20ml及び1Nの硝酸20mlを加えたものを加熱し、フェライト粒子を完全溶解させた水溶液を準備し、ICP分析装置(島津製作所製ICPS−1000IV)を用いてFe、Mg、Ti及びSrの含有量を測定した。
磁気特性は、振動試料型磁気測定装置(型式:VSM−C7−10A(東英工業社製))を用いて測定した。測定試料(フェライト粒子)は、内径5mm、高さ2mmのセルに詰めて上記装置にセットした。測定は、印加磁場を加え、5K・1000/4π・A/mまで掃引した。次いで、印加磁場を減少させ、記録紙上にヒステリシスカーブを作成した。このカーブのデータより印加磁場が5K・1000/4π・A/mにおける磁化を読み取った。また、残留磁化及び保磁力も同様に算出した。
この体積平均粒径は、レーザー回折散乱法により測定した。装置として日機装株式会社製マイクロトラック粒度分析計(Model9320−X100)を用いた。屈折率は2.42とし、25±5℃、湿度55±15%の環境下で測定を行った。ここで言う体積平均粒径(メジアン径)とは、体積分布モード、ふるい下表示での累積50%粒子径である。分散媒には水を用いた。
このBET比表面積の測定は、比表面積測定装置(型式:Macsorb HM model−1208(マウンテック社製))を用いた。測定試料を比表面積測定装置専用の標準サンプルセルに約5〜7g入れ、精密天秤で正確に秤量し、測定ポートに試料(フェライト粒子)をセットし、測定を開始した。測定は1点法で行い、測定終了時に試料の重量を入力すると、BET比表面積が自動的に算出される。なお、測定前に前処理として、測定試料を薬包紙に20g程度を取り分けた後、真空乾燥機で−0.1MPaまで脱気し−0.1MPa以下に真空度が到達していることを確認した後、200℃で2時間加熱した。
環境:温度;10〜30℃、湿度;相対湿度で20〜80% 結露なし
この電気抵抗は、下記によって測定される。
電極間間隔6.5mmで非磁性の平行平板電極(10mm×40mm)を対向させ、その間に、試料(フェライト粒子)200mgを秤量して充填する。磁石(表面磁束密度:1500Gauss、電極に接する磁石の面積:10mm×30mm)を平行平板電極に付けることにより電極間に試料を保持させ、50V、100V、250V、500V及び1000Vの電圧を印加し、それらの印加電圧における抵抗を絶縁抵抗計(SM−8210、東亜ディケーケー(株)製)にて測定した。
このフェライト粒子の細孔径及び細孔容積の測定は、次のようにして行われる。すなわち、水銀ポロシメーターPascal140とPascal240(ThermoFisher Scientific社製)を用いて測定した。ディラトメーターはCD3P(粉体用)を使用し、サンプルは複数の穴を開けた市販のゼラチン製カプセルに入れて、ディラトメーター内に入れた。Pascal140で脱気後、水銀を充填し低圧領域(0〜400kPa)を測定し、1st Runとした。次に再び脱気と低圧領域(0〜400kPa)の測定を行い、2nd Runとした。2nd Runの後、ディラトメーターと水銀とカプセルとサンプルを合わせた重量を測定した。次にPascal240で高圧領域(0.1MPa〜200MPa)を測定した。この高圧部の測定で得られた水銀圧入量をもって、フェライト粒子の細孔容積、細孔径分布及びピーク細孔径を求めた。また、細孔径を求める際には水銀の表面張力を480dyn/cm、接触角を141.3°として計算した。
次に、本発明に係るフェライト粒子の製造方法について説明する。
Fe、Mn及びMgの各化合物、さらに必要に応じてSr、Ti等の化合物を粉砕、混合、仮焼した後、ロッドミルで粉砕し、フェライト仮焼粉とする。
上記のようにして得られた被覆前フェライト粒子に被覆用TiO2粒子を添加し、混合ミルで混合し、フェライト粒子用原料とした。このフェライト粒子用原料を不活性雰囲気又は弱酸化性雰囲気、例えば窒素雰囲気下や酸素濃度が3体積%以下の窒素と酸素の混合ガス雰囲気下、850〜1230℃で加熱することにより焼成した。
本発明に係る触媒は、上記フェライト粒子を触媒担持体として触媒活性成分(触媒粒子)を担持させる。触媒活性成分としては金、銀、銅、白金、ロジウム、ルテニウム、パラジウム、ニッケル、コバルトから選ばれる1種類以上の金属コロイド粒子が好ましい。
[フェライト粒子の調製]
Fe2O3を100モル、MgCO3を10モル、Mn3O413.3モル及びSrCO3を1モルとなるように秤量し、さらに、還元剤としてカーボンブラックを原料重量に対して1.35重量%添加したものを混合、粉砕後、ローラーコンパクターでペレット化した。得られたペレットを980℃にて酸素濃度0体積%下の窒素雰囲気下、ロータリー式の焼成炉で仮焼成を行った。これをロッドミルにて粉砕したものをフェライト芯材用仮焼粉とした。
フェライト原料として、Fe2O3を100モル、MgCO3を5モル、Mn3O426.6モル及びSrCO3を0モルとなるように秤量した以外は、実施例1と同様の方法でフェライト粒子を得た。
フェライト原料として、Fe2O3を100モル、MgCO3を20モル、Mn3O46.65モル及びSrCO3を0モルとなるように秤量した以外は、実施例1と同様の方法でフェライト粒子を得た。
フェライト原料として、Fe2O3を100モル、MgCO3を5モル、Mn3O45モル、及びSrCO3を0モルとなるように秤量した以外は、実施例1と同様の方法でフェライト粒子を得た。
フェライト原料として、Fe2O3を100モル、MgCO3を20モル、Mn3O426.6モル及びSrCO3を0モルとなるように秤量した以外は、実施例1と同様の方法でフェライト粒子を得た。
SrCO3を0モルとし、被覆用TiO2粒子を、上記フェライト芯材用粒子に対して2.5重量%添加した以外は、実施例1と同様の方法でフェライト粒子を得た。
SrCO3を0モルとし、被覆用TiO2粒子を、上記フェライト芯材用粒子に対して5重量%添加した以外は、実施例1と同様の方法でフェライト粒子を得た。
本焼成温度を950℃とした以外は、実施例6と同様の方法でフェライト粒子を得た。
本焼成温度を1050℃とした以外は、実施例6と同様の方法でフェライト粒子を得た。
SrCO 3 を0モルとし、本焼成温度を920℃とした以外は、実施例1と同様の方法でフェライト粒子を得た。
SrCO 3 を0モルとし、被覆用TiO2粒子を、フェライト芯材用粒子に対して添加しなかった以外は、実施例1と同様の方法でフェライト粒子を得た。
SrCO 3 を0モルとし、本焼成温度を1165℃とした以外は、実施例1と同様の方法でフェライト粒子を得た。
[実施例10]
実施例1で得られたフェライト粒子に金コロイド溶液をコロイド粒子の重量がフェライト粒子の1重量%となるように含浸させ、コロイド溶液の溶媒を蒸発させたのち、イナートオーブンを用いて700℃、窒素雰囲気化で6時間熱処理を行った。熱処理後のフェライト粒子(触媒担持した状態のフェライト粒子)を樹脂に包埋したのち、イオンミリングにて粒子断面が見えるように加工した。EDXを用いて得られた粒子内部の元素の分布状態を確認した。
コロイド溶液を銀コロイド溶液とした以外は実施例10と同様の方法で触媒担持体粒子作製し、元素分布の状態を確認した。
コロイド溶液を銅コロイド溶液とした以外は実施例10と同様の方法で触媒担持体粒子作製し、元素分布の状態を確認した。
コロイド溶液を白金コロイド溶液とした以外は実施例10と同様の方法で触媒担持体粒子作製し、元素分布の状態を確認した。
コロイド溶液をロジウムコロイド溶液とした以外は実施例10と同様の方法で触媒担持体粒子作製し、元素分布の状態を確認した。
コロイド溶液をルテニウムコロイド溶液とした以外は実施例10と同様の方法で触媒担持体粒子作製し、元素分布の状態を確認した。
コロイド溶液をパラジウムコロイド溶液とした以外は実施例10と同様の方法で触媒担持体粒子作製し、元素分布の状態を確認した。
コロイド溶液をニッケルコロイド溶液とした以外は実施例10と同様の方法で触媒担持体粒子作製し、元素分布の状態を確認した。
コロイド溶液をコバルトコロイド溶液とした以外は実施例10と同様の方法で触媒担持体粒子作製し、元素分布の状態を確認した。
Claims (6)
- Tiが固溶されたフェライトを含む外殻構造を有し、
当該フェライト粒子内部に存在する細孔と当該外殻構造に存在する細孔とが連通し、
当該フェライト粒子内部に存在する細孔及び当該外殻構造に存在する細孔は、細孔容積が0.06〜0.2ml/gであり、ピーク細孔径は0.7〜2μmである
ことを特徴とする触媒担持体用フェライト粒子。 - 上記外殻構造を有する部分の厚さが0.5〜10μmである請求項1に記載の触媒担持体用フェライト粒子。
- 粒子内部の密度が上記外殻構造の密度より低い請求項1又は2に記載の触媒担持体用フェライト粒子。
- 体積平均粒径が10〜100μmである請求項1〜3のいずれかに記載の触媒担持体用フェライト粒子。
- 請求項1〜4のいずれかに記載のフェライト粒子を触媒担持体として用いた触媒。
- 触媒活性成分が金、銀、銅、白金、ロジウム、ルテニウム、パラジウム、ニッケル、コバルトから選ばれる1種類以上の金属コロイド粒子である請求項5記載の触媒。
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