JP7352910B2 - 機能性構造体及び機能性構造体の製造方法 - Google Patents
機能性構造体及び機能性構造体の製造方法 Download PDFInfo
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- JP7352910B2 JP7352910B2 JP2019521321A JP2019521321A JP7352910B2 JP 7352910 B2 JP7352910 B2 JP 7352910B2 JP 2019521321 A JP2019521321 A JP 2019521321A JP 2019521321 A JP2019521321 A JP 2019521321A JP 7352910 B2 JP7352910 B2 JP 7352910B2
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- IOWOAQVVLHHFTL-UHFFFAOYSA-N technetium(vii) oxide Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[Tc+7].[Tc+7] IOWOAQVVLHHFTL-UHFFFAOYSA-N 0.000 description 1
- LAJZODKXOMJMPK-UHFFFAOYSA-N tellurium dioxide Chemical compound O=[Te]=O LAJZODKXOMJMPK-UHFFFAOYSA-N 0.000 description 1
- IIXQANVWKBCLEB-UHFFFAOYSA-N tellurium trioxide Chemical compound O=[Te](=O)=O IIXQANVWKBCLEB-UHFFFAOYSA-N 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 238000004876 x-ray fluorescence Methods 0.000 description 1
- DRDVZXDWVBGGMH-UHFFFAOYSA-N zinc;sulfide Chemical compound [S-2].[Zn+2] DRDVZXDWVBGGMH-UHFFFAOYSA-N 0.000 description 1
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Description
[1]ゼオライト型化合物で構成される多孔質構造の骨格体と、前記骨格体に内在する少なくとも1つの固体酸と、を備え、前記骨格体が、互いに連通する通路を有し、前記固体酸が、前記骨格体の少なくとも前記通路に存在していることを特徴とする機能性構造体。
[2]前記通路は、拡径部を有し、かつ、前記固体酸は、少なくとも前記拡径部に包接されていることを特徴とする、[1]に記載の機能性構造体。
[3]前記拡径部は、前記一次元孔、前記二次元孔及び前記三次元孔のうちのいずれかを構成する複数の孔同士を連通している、[2]に記載の機能性構造体。
[4]前記固体酸は、触媒機能を有する微粒子であり、前記骨格体は、前記固体酸を担持する担体であることを特徴とする、[1]から[3]のいずれか1つに記載の機能性構造体。
[5]前記微粒子の平均粒径が、前記通路の平均内径よりも大きく、かつ、前記拡径部の内径以下であることを特徴とする、[4]に記載の機能性構造体。
[6]前記微粒子の平均粒径が、0.1nm~50nmであることを特徴とする、[4]又は[5]に記載の機能性構造体。
[7]前記微粒子の平均粒径が、0.45nm~14.0nmであることを特徴とする、[6]に記載の機能性構造体。
[8]前記通路の平均内径に対する前記微粒子の平均粒径の割合が、0.06~500であることを特徴とする、[1]~[7]のいずれか1つに記載の機能性構造体。
[9]前記通路の平均内径に対する前記微粒子の平均粒径の割合が、0.1~36であることを特徴とする、[8]に記載の機能性構造体。
[10]前記通路の平均内径に対する前記微粒子の平均粒径の割合が、1.7~4.5であることを特徴とする、[9]に記載の機能性構造体。
[11]前記固体酸が金属元素(M)を含有し、金属元素(M)が、前記機能性構造体に対して0.5~2.5質量%で含有されていることを特徴とする、請求項[1]から[10]のいずれか1つに記載の機能性構造体。
[12]前記通路は、前記ゼオライト型化合物の骨格構造によって画定される一次元孔、二次元孔及び三次元孔のうちのいずれかと、前記一次元孔、前記二次元孔及び前記三次元孔のうちのいずれとも異なる拡径部を有し、前記通路の平均内径は、0.1nm~1.5nmであり、前記拡径部の内径は、0.5nm~50nmであることを特徴とする、[1]~[11]のいずれか1つに記載の機能性構造体。
[13]前記骨格体の外表面に保持された少なくとも1つの機能性物質を更に備えることを特徴とする、[1]から[12]のいずれか1つに記載の機能性構造体。
[14]前記骨格体に内在する前記少なくとも1つの固体酸の含有量が、前記骨格体の外表面に保持された前記少なくとも1つの機能性物質の含有量よりも多いことを特徴とする、[13]に記載の機能性構造体。
[15]前記ゼオライト型化合物は、ケイ酸塩化合物であることを特徴とする、[1]~[14]のいずれか1つに記載の機能性構造体。
[16]ゼオライト型化合物で構成される多孔質構造の骨格体を得るための前駆体材料(A)に固体酸の金属含有溶液が含浸された前駆体材料(B)を焼成する焼成工程と、前記前駆体材料(B)を焼成して得られた前駆体材料(C)を水熱処理する水熱処理工程と、を有することを特徴とする機能性構造体の製造方法。
[17]前記焼成工程の前に、非イオン性界面活性剤を、前記前駆体材料(A)に対して50~500質量%添加することを特徴とする、[16]に記載の機能性構造体の製造方法。
[18]前記焼成工程の前に、前記前駆体材料(A)に前記金属含有溶液を複数回に分けて添加することで、前記前駆体材料(A)に前記金属含有溶液を含浸させることを特徴とする、[16]又は[17]に記載の機能性構造体の製造方法。
[19]前記焼成工程の前に前記前駆体材料(A)に前記金属含有溶液を含浸させる際に、前記前駆体材料(A)に添加する前記金属含有溶液の添加量を、前記前駆体材料(A)に添加する前記金属含有溶液中に含まれる金属元素(M)に対する、前記前駆体材料(A)を構成するケイ素(Si)の比(原子数比Si/M)に換算して、10~1000となるように調整することを特徴とする、[16]~[18]のいずれか1つに記載の機能性構造体の製造方法。
[20]前記水熱処理工程において、前記前駆体材料(C)と構造規定剤とを混合することを特徴とする、[16]に記載の機能性構造体の製造方法。
[21]前記水熱処理工程が塩基性雰囲気下で行われることを特徴とする、[16]に記載の機能性構造体の製造方法。
[機能性構造体の構成]
図1は、本発明の実施形態に係る機能性構造体の構成を概略的に示す図であり、(a)は斜視図(一部を横断面で示す。)、(b)は部分拡大断面図である。なお、図1における機能性構造体は、その一例を示すものであり、本発明に係る各構成の形状、寸法等は、図1のものに限られないものとする。
これにより、固体酸20の骨格体10内での移動がさらに規制され、固体酸20の離脱や、固体酸20、20同士の凝集をさらに有効に防止することができる。包接とは、固体酸20が骨格体10に内包されている状態を指す。このとき固体酸20と骨格体10とは、必ずしも直接的に互いが接触している必要はなく、固体酸20と骨格体10との間に他の物質(例えば、界面活性剤等)が介在した状態で、固体酸20が骨格体10に間接的に保持されていてもよい。
また、拡径部12は、上記一次元孔、上記二次元孔及び上記三次元孔のうちのいずれかを構成する複数の孔11a,11a同士を連通しているのが好ましい。これにより、骨格体10の内部に、一次元孔、二次元孔又は三次元孔とは異なる別途の通路が設けられるので、機能性物質20の機能をより発揮させることができる。
固体酸20が微粒子であるとき、微粒子は一次粒子の状態で通路11に存在している場合と、一次粒子が凝集して形成された二次粒子の状態で通路11に存在している場合とがある。いずれの場合においても、微粒子の平均粒径DCは、好ましくは通路11の平均内径DFよりも大きく、且つ拡径部12の内径DE以下である(DF<DC≦DE)。このような固体酸20は、通路11内では、好適には拡径部12に包接されており、骨格体10内での固体酸20の移動が規制される。よって、固体酸20が流体から外力を受けた場合であっても、骨格体10内での固体酸20の移動が抑制され、骨格体10の通路11に分散配置された拡径部12、12、・・のそれぞれに包接された固体酸20、20、・・同士が接触するのを有効に防止することができる。
また、固体酸20の金属元素(M)は、機能性構造体1に対して0.5~2.5質量%で含有されているのが好ましく、機能性構造体1に対して0.5~1.5質量%で含有されているのがより好ましい。例えば、金属元素(M)がZrである場合、Zr元素の含有量(質量%)は、(Zr元素の質量)/(機能性構造体1の全元素の質量)×100で表される。
機能性構造体1は、上記のとおり、多孔質構造の骨格体10と、骨格体に内在する少なくとも1つの固体酸20とを備える。機能性構造体1は、骨格体10に内在する固体酸20が流体と接触することにより、固体酸20の機能に応じた機能を発揮する。具体的に、機能性構造体1の外表面10aに接触した流体は、外表面10aに形成された孔11aから骨格体10内部に流入して通路11内に誘導され、通路11内を通って移動し、他の孔11aを通じて機能性構造体1の外部へ出る。流体が通路11内を通って移動する経路において、通路11に存在している固体酸20と接触することによって、固体酸20の機能に応じた反応(例えば、触媒反応)が生じる。また、機能性構造体1は、骨格体が多孔質構造であることにより、分子篩能を有する。
図3は、図1の機能性構造体1の製造方法を示すフローチャートである。以下、骨格体に内在する固体酸が金属酸化物微粒子である場合を例に、機能性構造体の製造方法の一例を説明する。
図3に示すように、先ず、ゼオライト型化合物で構成される多孔質構造の骨格体を得るための前駆体材料(A)を準備する。前駆体材料(A)は、好ましくは規則性メソ細孔物質であり、機能性構造体の骨格体を構成するゼオライト型化合物の種類(組成)に応じて適宜選択できる。
次に、準備した前駆体材料(A)に、金属含有溶液を含浸させ、前駆体材料(B)を得る。
次に、ゼオライト型化合物で構成される多孔質構造の骨格体を得るための前駆体材料(A)に金属含有溶液が含浸された前駆体材料(B)を焼成して、前駆体材料(C)を得る。
次いで、前駆体材料(C)と構造規定剤とを混合した混合溶液を調製し、前記前駆体材料(B)を焼成して得られた前駆体材料(C)を水熱処理して、機能性構造体を得る。
ここでの反応メカニズムは必ずしも明らかではないが、前駆体材料(C)を原料として水熱処理を行うことにより、前駆体材料(C)の規則性メソ細孔物質としての骨格構造は次第に崩れるが、前駆体材料(C)の細孔内部での金属酸化物微粒子の位置は概ね維持されたまま、構造規定剤の作用により、機能性構造体の骨格体としての新たな骨格構造(多孔質構造)が形成される。このようにして得られた機能性構造体は、多孔質構造の骨格体と、骨格体に内在する金属酸化物微粒子を備え、さらに骨格体はその多孔質構造により複数の孔が互いに連通した通路を有し、金属酸化物微粒子はその少なくとも一部分が骨格体の通路に保持されている。
また、本実施形態では、上記水熱処理工程において、前駆体材料(C)と構造規定剤とを混合した混合溶液を調製して、前駆体材料(C)を水熱処理しているが、これに限らず、前駆体材料(C)と構造規定剤とを混合すること無く、前駆体材料(C)を水熱処理してもよい。
図4は、図1の機能性構造体1の変形例を示す模式図である。
図1の機能性構造体1は、骨格体10と、骨格体10に内在する固体酸20とを備えるが、この構成だけに限定されず、例えば、図4に示すように、機能性構造体2が、骨格体10の外表面10aに保持された少なくとも1つの機能性物質30を更に備えていてもよい。
[前駆体材料(A)の合成]
シリカ剤(テトラエトキシシラン(TEOS)、和光純薬工業株式会社製)と、鋳型剤としての界面活性剤とを混合した混合水溶液を作製し、適宜pH調整を行い、密閉容器内で、80~350℃、100時間、水熱処理を行った。その後、生成した沈殿物をろ別し、水及びエタノールで洗浄し、さらに600℃、24時間、空気中で焼成して、表1~6に示す種類及び孔径の前駆体材料(A)を得た。なお、界面活性剤は、前駆体材料(A)の種類に応じて(「前駆体材料(A)の種類:界面活性剤」)以下のものを用いた。
・MCM-41:ヘキサデシルトリメチルアンモニウムブロミド(CTAB)(和光純薬工業株式会社製)
・SBA-1:Pluronic P123(BASF社製)
次に、表1~6に示す種類の固体酸微粒子を構成する金属元素(M)に応じて、該金属元素(M)を含有する金属塩を、水に溶解させて、金属含有水溶液を調製した。なお、金属塩は、固体酸微粒子の種類に応じて(「固体酸微粒子:金属塩」)以下のものを用いた。
・ZnOX:硝酸亜鉛六水和物(和光純薬工業株式会社製)
・AlOX:硝酸アルミニウム九水和物(和光純薬工業株式会社製)
・ZrOX:硝酸ジルコニル二水和物(和光純薬工業株式会社製)
上記のようにして得られた前駆体材料(C)と、表1~6に示す構造規定剤とを混合して混合水溶液を作製し、密閉容器内で、80~350℃、表1~6に示すpH及び時間の条件で、水熱処理を行った。その後、生成した沈殿物をろ別し、水洗し、100℃で12時間以上乾燥させ、さらに600℃、24時間、空気中で焼成して、表1~6に示す骨格体と機能性物質としての固体酸微粒子とを有する機能性構造体を得た(実施例1~288)。
比較例1では、MFI型シリカライトに平均粒径50nm以下の酸化コバルト粉末(II,III)(シグマ アルドリッチ ジャパン合同会社製)を混合し、骨格体としてのシリカライトの外表面に、機能性物質として酸化コバルト微粒子を付着させた機能性構造体を得た。MFI型シリカライトは、金属を添加する工程以外は、実施例52~57と同様の方法で合成した。
比較例2では、酸化コバルト微粒子を付着させる工程を省略したこと以外は、比較例1と同様の方法にてMFI型シリカライトを合成した。
実施例1~288及び比較例1~2のシリカライトについて、以下に示す条件で、各種特性評価を行った。
実施例1~288の機能性構造体及び比較例1~2のシリカライトについて、粉砕法にて観察試料を作製し、透過電子顕微鏡(TEM)(TITAN G2、FEI社製)を用いて、断面観察を行った。
また、上記実施例のうち固体酸微粒子がZrOxである機能性構造体について、FIB(集束イオンビーム)加工により断面を切り出し、SEM(SU8020、株式会社日立ハイテクノロジーズ製)、EDX(X-Max、株式会社堀場製作所製)を用いて断面元素分析を行った。その結果、骨格体内部からZr元素が検出された。
上記TEMとSEM/EDXによる断面観察の結果から、骨格体内部にZrOx微粒子が存在していることが確認された。
上記評価[A]で行った断面観察により撮影したTEM画像にて、骨格体の通路を、任意に500個選択し、それぞれの長径及び短径を測定し、その平均値からそれぞれの内径を算出し(N=500)、さらに内径の平均値を求めて、骨格体の通路の平均内径DFとした。また、固体酸微粒子についても同様に、上記TEM画像から、固体酸微粒子を、任意に500個選択し、それぞれの粒径を測定して(N=500)、その平均値を求めて、固体酸微粒子の平均粒径DCとした。結果を表1~6に示す。
また、機能性物質の平均粒径及び分散状態を確認するため、SAXS(小角X線散乱)を用いて分析した。SAXSによる測定は、Spring-8のビームラインBL19B2を用いて行った。得られたSAXSデータは、Guinier近似法により球形モデルでフィッティングを行い、粒径を算出した。粒径は、固体酸が酸化鉄微粒子である機能性構造体について測定した。また、比較対象として、市販品である酸化鉄微粒子(Wako製)をSEMにて観察、測定した。
この結果、市販品では粒径約50nm~400nmの範囲で様々なサイズの酸化鉄微粒子がランダムに存在しているのに対し、TEM画像から求めた平均粒径が1.2nm~2.0nmの各実施例の機能性構造体では、SAXSの測定結果においても粒径が10nm以下の散乱ピークが検出された。SAXSの測定結果とSEM/EDXによる断面の測定結果から、骨格体内部に、粒径10nm以下の機能性物質が、粒径が揃いかつ非常に高い分散状態で存在していることが分かった。
原子数比Si/M=50,100,200,1000(M=Al、Zr、Zn)の添加量で、固体酸を骨格体内部に包接させた機能性構造体を作製し、その後、上記添加量で作製された機能性構造体の骨格体内部に包接された金属量(質量%)を測定した。尚、本測定において原子数比Si/M=100,200,1000の機能性構造体は、それぞれ実施例1~288のうちの原子数比Si/M=100,200,1000の機能性構造体と同様の方法で金属含有溶液の添加量を調整して作製し、原子数比Si/M=50の機能性構造体は、金属含有溶液の添加量を異ならせたこと以外は、原子数比Si/M=100,200,1000の機能性構造体と同様の方法で作製した。
金属量の定量は、ICP(高周波誘導結合プラズマ)単体か、或いはICPとXRF(蛍光X線分析)を組み合わせて行った。XRF(エネルギー分散型蛍光X線分析装置「SEA1200VX」、エスエスアイ・ナノテクノロジー社製)は、真空雰囲気、加速電圧15kV(Crフィルター使用)或いは加速電圧50kV(Pbフィルター使用)の条件で行った。
XRFは、金属の存在量を蛍光強度で算出する方法であり、XRF単体では定量値(質量%換算)を算出できない。そこで、Si/M=100で金属を添加した機能性構造体の金属量は、ICP分析により定量し、Si/M=50および100未満で金属を添加した機能性構造体の金属量は、XRF測定結果とICP測定結果を元に算出した。
この結果、少なくとも原子数比Si/Mが50~1000の範囲内で、金属含有溶液の添加量の増加に伴って、機能性構造体に包接された金属量が増大していることが確認された。
実施例及び比較例の機能性構造体について、固体酸微粒子(触媒物質)がもつ触媒能(性能)を評価した。結果を表1~6に示す。
触媒活性は、以下の条件で評価した。
ル物質)の分解反応を行った。
10GC(サーモフィッシャーサイエンティフィック株式会社製、検出器:熱伝導度検出器)を用い、生成液の分析装置には、TRACE DSQ(サーモフィッシャーサイエン
ティフィック株式会社製、検出器:質量検出器、イオン化方法:EI(イオン源温度250℃、MSトランスファーライン温度320℃、検出器:熱伝導度検出器))を用いた。
耐久性は、以下の条件で評価した。
まず、評価(1)で使用した機能性構造体を回収し、650℃で、12時間加熱して、加熱後の機能性構造体を作製した。次に、得られた加熱後の機能性構造体を用いて、評価(1)と同様の方法により、ブチルベンゼン(重質油のモデル物質)の分解反応を行い、さらに評価(1)と同様の方法で、生成ガス及び生成液の成分を分析した。
その結果、各実施例において、前駆体材料(A)に添加する金属含有溶液の添加量が、原子数比Si/M(M=Zr)に換算して50~200(機能性構造体に対する固体酸の金属元素(M)の含有量が0.5~2.5質量%)であると、生成液中に含まれるブチルベンゼンよりも分子量が小さい化合物の収率が、32mol%以上となり、ブチルベンゼンの分解反応における触媒活性が合格レベル以上であることが分かった。
10 骨格体
10a 外表面
11 通路
11a 孔
12 拡径部
20 固体酸
30 機能性物質
Claims (18)
- ゼオライト型化合物で構成される多孔質構造の骨格体と、
前記骨格体に内在する少なくとも1つの固体酸と、
を備え、
前記骨格体が、互いに連通する通路を有し、
前記通路が、前記ゼオライト型化合物の骨格構造によって画定される一次元孔、二次元孔及び三次元孔のうちのいずれかと、前記一次元孔、前記二次元孔及び前記三次元孔のうちのいずれとも異なる拡径部を有し、
前記固体酸が、前記通路の少なくとも前記拡径部に包接されて存在しており、
前記固体酸の平均粒径が、前記通路の平均内径よりも大きく、かつ、前記拡径部の内径以下であり、ここで、前記通路の平均内径は、前記一次元孔、前記二次元孔及び前記三次元孔のうちのいずれかを構成する孔の短径及び長径の平均値から算出されるものであり、
前記固体酸が、酸化アルミニウム、酸化ジルコニウム及び酸化亜鉛からなる群から選択される少なくとも1種であり、
前記固体酸は、触媒機能を有する微粒子であり、前記通路の平均内径に対する前記微粒子の平均粒径の割合が、1.7~36であることを特徴とする機能性構造体。 - 前記拡径部は、前記一次元孔、前記二次元孔及び前記三次元孔のうちのいずれかを構成する複数の孔同士を連通している、請求項1に記載の機能性構造体。
- 前記骨格体は、前記固体酸を担持する担体であることを特徴とする、請求項1又は2に記載の機能性構造体。
- 前記微粒子の平均粒径が、0.1nm~50nmであることを特徴とする、請求項1~3のいずれか1項に記載の機能性構造体。
- 前記微粒子の平均粒径が、0.45nm~14.0nmであることを特徴とする、請求項4に記載の機能性構造体。
- 前記通路の平均内径に対する前記微粒子の平均粒径の割合が、1.7~35.7であることを特徴とする、請求項1~5のいずれか1項に記載の機能性構造体。
- 前記通路の平均内径に対する前記微粒子の平均粒径の割合が、1.7~17.9であることを特徴とする、請求項6に記載の機能性構造体。
- 前記通路の平均内径に対する前記微粒子の平均粒径の割合が、1.7~4.5であることを特徴とする、請求項7に記載の機能性構造体。
- 前記固体酸が金属元素(M)を含有し、金属元素(M)が、前記機能性構造体に対して0.5~2.5質量%で含有されていることを特徴とする、請求項1~8のいずれか1項に記載の機能性構造体。
- 前記通路の平均内径は、0.1nm~1.5nmであり、
前記拡径部の内径は、0.5nm~50nmであることを特徴とする、請求項1~9のいずれか1項に記載の機能性構造体。 - 前記骨格体の外表面に保持された少なくとも1つの機能性物質を更に備えることを特徴とする、請求項1~10のいずれか1項に記載の機能性構造体。
- 前記骨格体に内在する前記少なくとも1つの固体酸の含有量が、前記骨格体の外表面に保持された前記少なくとも1つの機能性物質の含有量よりも多いことを特徴とする、請求項11に記載の機能性構造体。
- 前記ゼオライト型化合物は、ケイ酸塩化合物であることを特徴とする、請求項1~12のいずれか1項に記載の機能性構造体。
- 規則性メソ細孔物質である前駆体材料(A)にアルミニウム、ジルコニウム及び亜鉛からなる群から選択される1種以上の金属元素に対応する金属成分を含む金属含有溶液が含浸された前駆体材料(B)を焼成する焼成工程と、
前記前駆体材料(B)を焼成して得られた前駆体材料(C)を水熱処理する水熱処理工程と、
を有する、固体酸を備える機能性構造体の製造方法であって、
前記固体酸が、酸化アルミニウム、酸化ジルコニウム及び酸化亜鉛からなる群から選択される少なくとも1種であり、
前記水熱処理工程において、前記前駆体材料(C)と構造規定剤とを混合して水熱処理することを特徴とする機能性構造体の製造方法。 - 前記焼成工程の前に、非イオン性界面活性剤を、前記前駆体材料(A)に対して50~500質量%添加することを特徴とする、請求項14に記載の機能性構造体の製造方法。
- 前記焼成工程の前に、前記前駆体材料(A)に前記金属含有溶液を複数回に分けて添加することで、前記前駆体材料(A)に前記金属含有溶液を含浸させることを特徴とする、請求項14又は15に記載の機能性構造体の製造方法。
- 前記焼成工程の前に前記前駆体材料(A)に前記金属含有溶液を含浸させる際に、前記前駆体材料(A)に添加する前記金属含有溶液の添加量を、前記前駆体材料(A)に添加する前記金属含有溶液中に含まれる金属元素(M)に対する、前記前駆体材料(A)を構成するケイ素(Si)の比(原子数比Si/M)に換算して、10~1000となるように調整することを特徴とする、請求項14~16のいずれか1項に記載の機能性構造体の製造方法。
- 前記水熱処理工程が塩基性雰囲気下で行われることを特徴とする、請求項14に記載の機能性構造体の製造方法。
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EP3632549A4 (en) | 2021-03-03 |
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WO2018221693A1 (ja) | 2018-12-06 |
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