JP6978783B2 - 金属有機構造体ナノシートおよびその製造方法 - Google Patents
金属有機構造体ナノシートおよびその製造方法 Download PDFInfo
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- JP6978783B2 JP6978783B2 JP2018528913A JP2018528913A JP6978783B2 JP 6978783 B2 JP6978783 B2 JP 6978783B2 JP 2018528913 A JP2018528913 A JP 2018528913A JP 2018528913 A JP2018528913 A JP 2018528913A JP 6978783 B2 JP6978783 B2 JP 6978783B2
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- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 54
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- 230000002209 hydrophobic effect Effects 0.000 claims description 27
- 229910052757 nitrogen Inorganic materials 0.000 claims description 26
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- SNGREZUHAYWORS-UHFFFAOYSA-N perfluorooctanoic acid Chemical compound OC(=O)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)F SNGREZUHAYWORS-UHFFFAOYSA-N 0.000 description 1
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- DCBSHORRWZKAKO-UHFFFAOYSA-N rac-1-monomyristoylglycerol Chemical compound CCCCCCCCCCCCCC(=O)OCC(O)CO DCBSHORRWZKAKO-UHFFFAOYSA-N 0.000 description 1
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Images
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/223—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material containing metals, e.g. organo-metallic compounds, coordination complexes
- B01J20/226—Coordination polymers, e.g. metal-organic frameworks [MOF], zeolitic imidazolate frameworks [ZIF]
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- B—PERFORMING OPERATIONS; TRANSPORTING
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Description
[1]1の二分子膜を構成する2つの単分子層の間にシート状に配置された金属有機構造体を備え、複数の前記二分子膜が溶媒中で超膨潤ラメラ相をなす、金属有機構造体ナノシート。
[2]前記二分子膜が、非イオン性両親媒性物質から構成される、前記[1]に記載の金属有機構造体ナノシート。
[3]非イオン性両親媒性物質が、エステル型界面活性剤、エーテル型界面活性剤、エステルエーテル型界面活性剤、アルカノールアミド型界面活性剤、アルキルグリコシド、高級アルコールからなる群より選ばれる少なくとも1種である、前記[2]に記載の金属有機構造体ナノシート。
[4]非イオン性両親媒性物質が、エーテル型界面活性剤であり、前記エーテル型界面活性剤が、ポリエチレングリコールモノアルキルエーテルおよびポリオキシエチレンアルキルフェニルエーテルからなる群より選ばれる少なくとも1種である、前記[3]に記載の金属有機構造体ナノシート。
[5]前記二分子膜が、下記式(1)
で示されるポリエチレングリコールモノアルキルエーテルから構成される、前記[1]に記載の金属有機構造体ナノシート。
[6]2<n/m<6である、前記[5]に記載の金属有機構造体ナノシート。
[7]nが12であり、mが5である、前記[5]に記載の金属有機構造体ナノシート。
[8]前記溶媒が、水または水と水溶性有機溶媒との混合液を含む、前記[1]〜[6]のいずれかに記載の金属有機構造体ナノシート。
[9]nが12であり、mが6であり、さらに前記溶媒が水と有機溶媒とを含む、前記[5]に記載の金属有機構造体ナノシート。
[10]前記金属有機構造体が、親油性が高い配位子を構成成分とする金属有機構造体である、前記[6]〜[9]のいずれかに記載の金属有機構造体ナノシート。
[11]超膨潤ラメラ相が、隣接する二分子膜間の距離が50nm以上のラメラ構造を有する、前記[1]〜[10]のいずれかに記載の金属有機構造体ナノシート。
[12]液体中において分散状態にある金属有機構造体ナノシートを含み、前記金属有機構造体ナノシートは、前記[1]〜[11]のいずれかに記載の金属有機構造体ナノシートである、金属有機構造体ナノシート分散液。
[13]溶媒中に二分子膜が超膨潤ラメラ相をなす場合において、1の二分子膜を構成する2つの単分子層の間にナノシートを形成する、ナノシートの製造方法。
[14]ナノシートが金属有機構造体から構成される、前記[13]に記載のナノシートの製造方法。
[15]溶媒中に二分子膜を形成し、前記溶媒中に有機配位子を添加して、二分子膜の超膨潤ラメラ相を形成し、その後、前記溶媒中に金属イオンを添加して、1の前記二分子膜を構成する2つの単分子層の間に金属有機構造体ナノシートを形成する、前記[14]に記載のナノシートの製造方法。
[16]前記二分子膜を構成する2つの単分子層の間に金属有機構造体ナノシートを形成した後に、前記二分子膜を除去する、前記[14]または[15]に記載のナノシートの製造方法。
[17]前記二分子膜が、下記式(1)
で示されるポリエチレングリコールモノアルキルエーテルで構成される、前記[14]〜[16]のいずれかに記載のナノシートの製造方法。
[18]2<n/m<6である、前記[17]に記載のナノシートの製造方法。
[19]nが12であり、mが5である、前記[17]に記載のナノシートの製造方法。
[20]前記溶媒が水または水と水溶性有機溶媒との混合液とを含む、前記[15]〜[19]のいずれかに記載のナノシートの製造方法。
[21]nが12であり、mが6であり、さらに前記溶媒が水と有機溶媒とを含む、前記[17]に記載のナノシートの製造方法。
[22]前記金属有機構造体が、親油性が高い配位子を構成成分とする金属有機構造体である、前記[14]〜[21]のいずれかに記載のナノシートの製造方法。
[23]ナノシートが金属酸化物または金属から構成される、前記[13]に記載のナノシートの製造方法。
[24]溶媒中に二分子膜を形成し、前記溶媒中に両親媒性物質を添加して、二分子膜の超膨潤ラメラ相を形成し、その後、前記溶媒中に酸素原子を有する金属含有化合物または酸素原子を有しない金属含有化合物を添加して、1の前記二分子膜を構成する2つの単分子層の間に金属酸化物ナノシートまたは金属ナノシートを形成する、前記[23]に記載のナノシートの製造方法。
[25]前記溶媒が、水と有機溶媒との混合液を含む、前記[24]に記載のナノシートの製造方法。
[26]さらに、前記溶媒中に界面活性助剤を添加する、前記[24]または[25]に記載のナノシートの製造方法。
[27]両親媒性物質が、陰イオン性両親媒性物質である、前記[24]〜[26]のいずれかに記載のナノシートの製造方法。
[28]前記[1]〜[11]のいずれかに記載の金属有機構造体ナノシートを含む、ガス分離膜。
[29]窒素分離用または二酸化炭素分離用である、前記[28]に記載のガス分離膜。
[30]1の二分子膜を構成する2つの単分子層の間にシート状に配置された金属酸化物を備え、複数の前記二分子膜が溶媒中で超膨潤ラメラ相をなす、金属酸化物ナノシート。
[31]1の二分子膜を構成する2つの単分子層の間にシート状に配置された金化合物を備え、複数の前記二分子膜が溶媒中で超膨潤ラメラ相をなす、金ナノシート。
本開示の第1実施形態にかかる金属有機構造体ナノシートは、1の二分子膜を構成する2つの単分子層の間にシート状に配置された金属有機構造体を備え、複数の二分子膜が溶媒中で超膨潤ラメラ相をなす。
で示されるポリエチレングリコールモノアルキルエーテル(CnEm)を含むポリエチレングリコールモノアルキルエーテル;下記式(2)
第2実施形態にかかる金属有機構造体ナノシート分散液は、液体中において分散状態にある金属有機構造体ナノシートを含み、前記金属有機構造体ナノシートは、上記いずれかの第1実施形態にかかる金属有機構造体ナノシートである。
第3実施形態にかかるナノシートの製造方法は、溶媒中に二分子膜が超膨潤ラメラ相をなす場合において、1の二分子膜を構成する2つの単分子層の間にナノシートを形成する工程を備える。
また、本開示にかかる他の実施形態としては、上記したいずれかの金属有機構造体ナノシートを含むガス分離膜が挙げられる。前記ガス分離膜は、窒素分離用または二酸化炭素分離用であってもよい。また、ガス分離膜は、複数の上記したいずれかの金属有機構造体ナノシートを積層した多層構造体であってもよく、複数の上記したいずれかの金属有機構造体ナノシートと公知のガス分離膜とを積層した複合構造体であってもよい。ガス分離膜の厚さは、目的に応じて、種々変更することができる。
また、本開示にかかる他の実施形態としては、1の二分子膜を構成する2つの単分子層の間にシート状に配置された金属酸化物を備え、複数の前記二分子膜が溶媒中で超膨潤ラメラ相をなす、金属酸化物ナノシートが挙げられる。さらに、本開示にかかる他の実施形態としては、1の二分子膜を構成する2つの単分子層の間にシート状に配置された金属(例えば、金、ニッケル)を備え、複数の前記二分子膜が溶媒中で超膨潤ラメラ相をなす、金属ナノシート(例えば、金ナノシート、ニッケルナノシート)が挙げられる。他の実施形態としては、金属酸化物ナノシートと、両親媒性物質とから構成される二分子膜とを備える複合ナノシートが挙げられる。また、金属ナノシートと、両親媒性物質とから構成される二分子膜とを備える複合ナノシートが挙げられる。
原子間力顕微鏡:東陽テクニカ社製、NanoScope III TappingMode AFM
走査型電子顕微鏡(SEM):日立製作所社製 S−5000
透過型電子顕微鏡(TEM):日立製作所社製 H−800
(X線回折スペクトル測定)
X線回折装置:リガク社製、MiniFlex II diffractometer
X線源 :CuKα
管球電圧:30kV
管球電流:15mA
(気体吸着量測定)
高精度ガス/蒸気吸着量測定装置 :マイクロトラック・ベル社製 BELSORP−max
測定温度;77K
吸着ガス純度:窒素及び二酸化炭素ともに99.99体積%
測定試料 前処理方法
サンプルを約30mg秤量し、真空下(P<10-4Pa)、373K、2時間静置。
金属有機構造体としてELM−11([Cu(bpy)2(BF4)2])を用いた金属有機構造体ナノシートを、以下の方法で調製した。
ELM−13を金属有機構造体として用いたナノシート(以下、ELM−13ナノシート)およびバルクの金属有機構造体であるELM−13(以下、バルクELM−13)を調製し、両者について窒素吸着量の圧力依存性を測定した。
試験管にCu(BF4)水溶液(80mM、6.25mL)を入れ,KCF3BF3(1.0mmol)を加えて溶かした。ここに4,4’−ビピリジン(bpy)のアセトン溶液(80mM、12.5mL)をゆっくりと滴下し、ELM−13を積層した。これを2週間静置した後、析出した青色結晶を減圧濾過し、減圧乾燥し、青色の高分子金属錯体の結晶を得た。
ポリエチレングリコールモノアルキルエーテル(CnEm)について、疎水部のアルキル基の炭素数および親水部のエチレンオキサイド数を変化させた場合の、超膨潤ラメラ相形成の有無を検討した。
第2実験例では、ポリエチレングリコールモノアルキルエーテル(CnEm)について、疎水部のアルキル基の炭素数および親水部のエチレンオキサイド数を変化させた場合の、超膨潤ラメラ相の形成温度を比較した。
第3実験例では、トルエン−水系において、ポリエチレングリコールモノアルキルエーテル(C12E6)が超膨潤ラメラ相を形成するための、トルエンおよびC12E6の含量条件について検討した。
第4実験例では、ポリエチレングリコールモノアルキルエーテル(C12E5ないしC12E6)にグリセリンを添加した場合の、超膨潤ラメラ相の形成温度を比較した。
20mLスクリュー管瓶にC12E5、グリセリンおよび脱イオン水を混合し、様々なグリセリン濃度の溶液を調製した。それぞれの溶液を撹拌、加熱しながら、溶液の色の変化の観察を行った。また、呈色が確認できた温度において、C12E5水溶液と同様に反射スペクトルの測定を行った。C12E5の濃度が2質量%となる溶液については、粘度測定も行った。
20mLスクリュー管瓶にC12E6、トルエン、グリセリンおよび脱イオン水を混合し、様々なグリセリン濃度の溶液を調製した。それぞれの溶液を撹拌、加熱しながら、溶液の色の変化の観察を行った。なお、C12E6とトルエンはそれぞれ系全体で2質量%および0.67質量%となるように調製した。結果を図14及び図15に示した。
図14及び図15に示すように、グリセリン添加量の増加に伴って、超膨潤ラメラ相の形成温度は低下する。グリセリン添加量の増加に伴って、系(溶液)の濃度が上昇し、ヘルフリッヒ(Helfrich)相互作用が変化し、超膨潤ラメラ相の形成温度は低下するものと考えられる。このことから、グリセリンの添加により、超膨潤ラメラ相の形成温度を制御可能であることが分かった。
第5実験例では、ポリエチレングリコールモノアルキルエーテル(C12E5ないしC12E6)の含量を変化させた場合の、超膨潤ラメラ相における層間距離(隣接する二分子膜間の間隔:図1A及び図1BにおけるD)を比較した。
第6実験例では、グリセリンの含量を変化させた場合の、超膨潤ラメラ相における層間距離(隣接する二分子膜間の間隔:図1A及び図1BにおけるD)を比較した。
20mLスクリュー管瓶に、n−デカン9.2g(89.8質量%)、1−ペンタノール0.85g(8.3質量%)、オクチルベンゼンスルホン酸ナトリウム0.09g(0.9質量%)、水0.1g(1.0質量%)となるように、各成分を添加して混合し、界面活性剤溶液を調製した。10.2gの前記界面活性剤溶液に、シリカ原料としてテトラエトキシシラン(TEOS;和光純薬社製)を0.074g添加し、混合溶液を得た。この混合溶液を長さ20mm、直径7mmのマグネチックスターラーを用いて常温で72時間、300rpmで撹拌し、超膨潤ラメラ相が安定的に維持されていることを確認した。シリカナノシートが生成された。得られたシリカナノシートは、溶液中に分散しており、この分散液に対して、洗浄操作を行い、シリカナノシートを単離した。前記洗浄操作としては、まず、前記分散液を用いて遠心分離し、得られた固形分にメタノールを加えて遠心分離をし、上清を捨て、再度メタノールを加えて遠心分離をし、上清を捨てた。この洗浄操作を数回繰り返し、十分に洗浄を行った後で、残った固体を90℃で一晩乾燥させた。得られたシリカナノシートを透過型電子顕微鏡(TEM)で観察した結果を図18に示す。なお前記TEM観察時の観測倍率は12万倍、加速電圧は200KVであった。図18から、シリカナノシートが生成されたことが確認された。
実施例3に記載の界面活性剤溶液を、実施例3と同様に調製し、10.2gの前記界面活性剤溶液に、原料の金含有化合物としてテトラクロロ金(III)酸四水和物(HAuCl4・H2O;和光純薬社製)を10mg添加し、さらに塩化鉄(III)(和光純薬社製)1mgを添加して、混合溶液を得た。超膨潤ラメラ相が安定的に維持されていることを確認しつつ、この混合溶液に、UV照射装置(製品名:300Wキセノン光源、型番:MAX-303、朝日分光株式会社製)を用いてUV(波長350nm)を1時間照射し、金ナノシートを合成した。得られた金ナノシートは、溶液中に分散しており、この分散液に対して、洗浄操作を行い、金ナノシートを単離した。洗浄操作は実施例3と同様に行った。この洗浄操作を数回繰り返し、十分に洗浄を行った後で、残った固体を90℃で一晩乾燥させた。得られた金ナノシートを透過型電子顕微鏡で観察した結果を図19に示す。なお前記TEM観察時の観測倍率は1万倍、加速電圧は200KVであった。また、得られた金ナノシートを走査型電子顕微鏡(SEM)で観察した結果を図20に示す。なお前記SEM観察時の観測倍率は50万倍、加速電圧は15KVであった。図19および図20に示されるように、金ナノシートが生成されたことが確認された。TEM画像から、金ナノシートの横幅が約4μmであることが確認された。また、SEM画像から、金ナノシートの厚さが約6nmであることが確認された。
11 複合ナノシート
12 金ナノシート
3 溶媒
5 両親媒性分子
5A 溶媒に親和的な部分
5B 溶媒に非親和的な部分
10 二分子膜
20 スクリュー管
22 光源
24 分光器
Claims (31)
- 1の二分子膜を構成する2つの単分子層と、該単分子層の間にシート状に配置された状態にある金属有機構造体からなる複合ナノシートであり、
前記1の二分子膜は、他の前記1の二分子膜と共に溶媒中で超膨潤ラメラ相を形成する物質から構成される二分子膜であり、
前記超膨潤ラメラ相は、複数の二分子膜が溶媒の層を挟んで層状に積み重なった相である、
複合ナノシート。 - 前記二分子膜が、非イオン性両親媒性物質から構成される、請求項1に記載の複合ナノシート。
- 非イオン性両親媒性物質が、エステル型界面活性剤、エーテル型界面活性剤、エステルエーテル型界面活性剤、アルカノールアミド型界面活性剤、アルキルグリコシド、高級アルコールからなる群より選ばれる少なくとも1種である、請求項2に記載の複合ナノシート。
- 非イオン性両親媒性物質が、エーテル型界面活性剤であり、前記エーテル型界面活性剤が、ポリエチレングリコールモノアルキルエーテルおよびポリオキシエチレンアルキルフェニルエーテルからなる群より選ばれる少なくとも1種である、請求項3に記載の複合ナノシート。
- 2<n/m<6である、請求項5に記載の複合ナノシート。
- nが12であり、mが5である、請求項5に記載の複合ナノシート。
- 前記溶媒が、水または水と水溶性有機溶媒との混合液を含む、請求項1〜6のいずれか1項に記載の複合ナノシート。
- nが12であり、mが6であり、さらに前記溶媒が水と有機溶媒とを含む、請求項5に記載の複合ナノシート。
- 前記金属有機構造体が、親油性が高い配位子を構成成分とする金属有機構造体である、請求項6〜9のいずれか1項に記載の複合ナノシート。
- 超膨潤ラメラ相が、隣接する二分子膜間の距離が50nm以上のラメラ構造を有する、請求項1〜10のいずれか1項に記載の複合ナノシート。
- 請求項1〜11のいずれか1項に記載の複合ナノシートと液体とを含み、
前記複合ナノシートが、液体中において分散状態である、
複合ナノシート分散液。 - 溶媒中で、二分子膜が前記溶媒の層を挟んで層状に積み重なった相である超膨潤ラメラ相を形成し、
1の二分子膜を構成する2つの単分子層の間にナノシートを形成する、
ナノシートの製造方法。 - ナノシートが金属有機構造体から構成される、請求項13に記載のナノシートの製造方法。
- 溶媒中に二分子膜を形成し、
前記溶媒中に有機配位子を添加して、二分子膜の超膨潤ラメラ相を形成し、
その後、前記溶媒中に金属イオンを添加して、1の前記二分子膜を構成する2つの単分子層の間に金属有機構造体ナノシートを形成する、請求項14に記載のナノシートの製造方法。 - 1の前記二分子膜を構成する2つの単分子層の間に金属有機構造体ナノシートを形成した後に、前記二分子膜を除去する、請求項14または15に記載のナノシートの製造方法。
- 2<n/m<6である、請求項17に記載のナノシートの製造方法。
- nが12であり、mが5である、請求項17に記載のナノシートの製造方法。
- 前記溶媒が水または水と水溶性有機溶媒との混合液とを含む、請求項15〜19のいずれか1項に記載のナノシートの製造方法。
- nが12であり、mが6であり、さらに前記溶媒が水と有機溶媒とを含む、請求項17に記載のナノシートの製造方法。
- 前記金属有機構造体が、親油性が高い配位子を構成成分とする金属有機構造体である、請求項14〜21のいずれか1項に記載のナノシートの製造方法。
- ナノシートが金属酸化物または金属から構成される、請求項13に記載のナノシートの製造方法。
- 溶媒中に二分子膜を形成し、
前記溶媒中に両親媒性物質を添加して、二分子膜の超膨潤ラメラ相を形成し、
その後、前記溶媒中に酸素原子を有する金属含有化合物または酸素原子を有しない金属含有化合物を添加して、1の前記二分子膜を構成する2つの単分子層の間に金属酸化物ナノシートまたは金属ナノシートを形成する、請求項23に記載のナノシートの製造方法。 - 前記溶媒が、水と有機溶媒との混合液を含む、請求項24に記載のナノシートの製造方法。
- さらに、前記溶媒中に界面活性助剤を添加する、請求項24または25に記載のナノシートの製造方法。
- 両親媒性物質が、陰イオン性両親媒性物質である、請求項24〜26のいずれか1項に記載のナノシートの製造方法。
- 請求項1〜11のいずれか1項に記載の複合ナノシートを含む、ガス分離膜。
- 窒素分離用または二酸化炭素分離用である、請求項28に記載のガス分離膜。
- 1の二分子膜を構成する2つの単分子層と、該単分子層の間にシート状に配置された状態にある金属酸化物からなる複合ナノシートであり、
前記1の二分子膜は、他の前記1の二分子膜と共に溶媒中で超膨潤ラメラ相を形成する物質から構成される二分子膜であり、
前記超膨潤ラメラ相は、複数の二分子膜が溶媒の層を挟んで層状に積み重なった相である、
複合ナノシート。 - 1の二分子膜を構成する2つの単分子層と、該単分子層の間にシート状に配置された状態にある金化合物からなる複合ナノシートであり、
前記1の二分子膜は、他の前記1の二分子膜と共に溶媒中で超膨潤ラメラ相を形成する物質から構成される二分子膜であり、
前記超膨潤ラメラ相は、複数の二分子膜が溶媒の層を挟んで層状に積み重なった相である、
複合ナノシート。
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