JP2013521212A - 高表面積の繊維状シリカナノ粒子 - Google Patents
高表面積の繊維状シリカナノ粒子 Download PDFInfo
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- JP2013521212A JP2013521212A JP2012555502A JP2012555502A JP2013521212A JP 2013521212 A JP2013521212 A JP 2013521212A JP 2012555502 A JP2012555502 A JP 2012555502A JP 2012555502 A JP2012555502 A JP 2012555502A JP 2013521212 A JP2013521212 A JP 2013521212A
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- nanoparticles
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- metal
- silica
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- 239000002105 nanoparticle Substances 0.000 title claims abstract description 157
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims description 165
- 239000000377 silicon dioxide Substances 0.000 title claims description 80
- 239000000835 fiber Substances 0.000 claims abstract description 85
- 238000004519 manufacturing process Methods 0.000 claims abstract description 9
- 238000000034 method Methods 0.000 claims description 46
- 239000002077 nanosphere Substances 0.000 claims description 40
- 229910052751 metal Inorganic materials 0.000 claims description 39
- 239000002184 metal Substances 0.000 claims description 39
- 239000000203 mixture Substances 0.000 claims description 37
- 239000003446 ligand Substances 0.000 claims description 34
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 33
- 239000003054 catalyst Substances 0.000 claims description 33
- 239000002904 solvent Substances 0.000 claims description 28
- -1 carbine Chemical group 0.000 claims description 21
- 229910044991 metal oxide Inorganic materials 0.000 claims description 20
- 150000004706 metal oxides Chemical class 0.000 claims description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 20
- 229910001868 water Inorganic materials 0.000 claims description 19
- 239000004202 carbamide Substances 0.000 claims description 17
- 239000002245 particle Substances 0.000 claims description 17
- 239000003814 drug Substances 0.000 claims description 15
- 239000002243 precursor Substances 0.000 claims description 15
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- 229910052739 hydrogen Inorganic materials 0.000 claims description 13
- 238000001354 calcination Methods 0.000 claims description 12
- QAQSNXHKHKONNS-UHFFFAOYSA-N 1-ethyl-2-hydroxy-4-methyl-6-oxopyridine-3-carboxamide Chemical group CCN1C(O)=C(C(N)=O)C(C)=CC1=O QAQSNXHKHKONNS-UHFFFAOYSA-N 0.000 claims description 8
- 229910052794 bromium Inorganic materials 0.000 claims description 8
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- 125000000058 cyclopentadienyl group Chemical group C1(=CC=CC1)* 0.000 claims description 3
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 claims description 3
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- 239000000126 substance Substances 0.000 description 8
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- 235000012239 silicon dioxide Nutrition 0.000 description 7
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 6
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- 150000001450 anions Chemical class 0.000 description 4
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 4
- 229910052710 silicon Inorganic materials 0.000 description 4
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 description 3
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- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
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- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
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Images
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Abstract
Description
本発明は概して、高表面積ナノ粒子及びその適用の分野に関連する。
2. 関連する技術の説明
ナノテクノロジーは、材料、マイクロエレクトロニクス、コンピューティング、製薬、医薬、環境、エネルギー及び化学産業に、大きな影響を与えている。ナノ粒子は、長い間、バルク型と比較して、より高められた化学的及び物理的特性を備えているものと認識されてきた。これらは、高い価値を有する材料の組み合わせを製造するための基礎的要素として適用されうる(Xia et al., 2000)。これらは、種々のサイズ、結晶化度、形態、及び化学組成物であり得る。ナノ粒子は種々の材料から構成され得、シリカが最もよく知られる例の一つである(例えば、Gole et al., 2003参照)。多数の産業上の利用のために、シリカナノ粒子、特に特定の寸法及び形態を有するナノ球体の必要性が増している。
(a) シリカ前駆体、テンプレート分子、及び溶媒を含む組成物を準備する工程であって、テンプレート分子が下記の構造式の化合物であり:
式中、nが5〜25の範囲の数字であり、かつR1が、
または
または
であり、式中、X-が、Cl、Br、I、またはFであり;かつR2〜R14がそれぞれ独立して、H、Cl、Br、I、OH、及びC1-C10アルキルからなる群より選択される、工程;
(b)(a)の組成物を熱またはマイクロ波照射にさらす工程であって、シリカを含む粒子が形成される、工程;及び
(c)溶媒の一部分またはすべてを(b)の組成物から取り除き、単離されたシリカテンプレート粒子を生産する工程;及び
(d)(c)の単離されたシリカテンプレート粒子をか焼させ、ナノ粒子を生産する工程。
本発明は、多孔性表面形態によって高表面積を有する、新しいクラスのナノ粒子の製造に基づく。ナノ粒子は、触媒、医薬送達及びクロマトグラフィーのような幅広い範囲の適用が可能となるように、表面と結合した分子の提示を可能にする。
本発明のいくつかの態様は、本発明のナノ粒子を製造する方法に関連する。
本発明のナノ粒子は、当業者に公知の任意の材料を使用して製造されうる。特定の態様では、シリカ前駆体を含むミクロエマルジョンが形成され、シリカから構成されるナノ粒子になる。
いくつかの態様において、ナノ粒子は、金属または金属酸化物のようなリガンドでコーティングされる。触媒であるリガンドとして使用される金属の例は、Fe、Cr、Al、Ga、In、Hf、Sn、Zr、Mo、Ti、V、Co、Ni、Cu、Y、Ta、W、Pb、B、Nb、Ge、Pr、U、Ce、ErNd、Mg、Ca、Ba、Sr、Au、Siまたはそれらの組み合わせを含むが、これに限定されない。さらに、金属酸化物ベースの材料が企図され、ケイ素、ゲルマニウム、すず、鉛、アンチモン、ビスマス、ポロニウム、ランタノイド、及びアクチナイドに基づく金属酸化物が含まれる。金属非酸化物ナノ粒子は、II-VI、III-V、及びIV量子ドットを含み;金属酸化物ナノ粒子は、酸化チタン、酸化ジルコニウム、酸化アルミニウム、酸化鉄、酸化タングステン、酸化セリウム、酸化アンチモン、及び酸化ケイ素を含みうる。金属酸化物の合成は、Fe3+、Cr3+、A3+、Ga3+、In3+、Hf4+、Sn4+、Zr4+、Nb5+、W6+、Pr3+、Er3+、Nd3+、Ce3+、U3+、Y3+及びそれらの組み合わせの塩のような無機塩を用いて行われてきている。
本発明のいくつかの態様は、金属以外に一種または複数種のリガンドが付着したナノ粒子に関する。リガンドの例は、有機分子及び医薬を含む。またリガンドとして企図されるのは、半導体材料及びセラミックである。セラミック材料のいくつかの例は、ブルシャイト、リン酸三カルシウム、アルミナ、シリカ、及びジルコニアを含む。いくつかの態様では、リガンドはポリマーである。ポリマーの例は、ポリスチレン、シリコンゴム、ポリカーボネート、ポリウレタン、ポリプロピレン、ポリメタクリル酸メチル、ポリ塩化ビニル、ポリエステル、ポリエーテル、及びポリエチレンを含む。生物分解性の、バイオポリマー(例えば、BSAなどのポリペプチド、多糖等)、他の生物学的材料(例えば、炭水化物)、及び/または重合体化合物が、可能なリガンドとして企図される。金もまた、その周知の反応性の特性及び生物学的不活性ゆえに、リガンドとして企図される。
本発明のナノ粒子は、リガンドが容易にその表面に結合できるように、表面改質され得る。ナノ粒子の表面改質は、例えば、ナノ粒子溶液を、カップリング剤(リンカー)を含む溶液で処理することによって達成されうる。例えば、カップリング剤は、シランカップリング剤でありうる。
ナノ粒子の形状には特に限定はなく、例えば、球状の、不規則な、細長い、楕円体、杆状体、三角形、六角形、等の形状であってよく、または少なくとも二つ以上の形状を含む組み合わせであってもよい。特定の態様では、ナノ粒子は、本質的に球状(すなわちナノ球体)である。
組成物の溶液において、ナノ粒子は概して、溶液の総重量に対して約0.0000001wt%〜約100wt%の量(塊がない粉末(solid-free powder))で溶液中に存在しうる。一つの態様において、ナノ粒子は概して、約0.000001wt%〜約15wt%の量で溶液中に存在しうる。別の態様では、ナノ粒子は概して、約0.01wt%〜約1wt%の量で溶液中に存在しうる。さらに別の態様では、ナノ粒子は概して、約1wt%〜約10wt%の量で溶液中に存在しうる。
いくつかの態様において、ナノ粒子は、プラスまたはマイナスの電荷を与えるように分子によって官能基化されうる。またナノ粒子は、疎水性または親水性の表面を提供するように分子によって官能基化されうる。
本発明のナノ粒子は、幅広い用途に用いられうる。例えば、上述のように、それらは、触媒または触媒支持体として用いられうる。それらはまた、水及び油から金属を除去するために用いられうる。それらはさらに、水素などのエネルギー貯蔵のために用いられうる。それらは、包装材料として包装産業で用いられうる。それらはまた、医薬送達、遺伝子送達、及び医薬イメージングにおいて利用されうる。ナノ粒子は、触媒、薬剤の輸送、医薬送達、包装、センサーとして、及びそれらの組み合わせにおいて利用されうる。本発明において有用な医薬は、治療化合物、放射性化合物、化学療法剤、DNA/RNA分子、タンパク質、またはMRI造影剤であり得る。
本発明のある態様は概して、本発明のナノ粒子を含むキットに関連する。例えばいくつかの態様において、キットは、一つまたは複数の、本明細書で述べたようなあらかじめ決められた量のナノ粒子を含むシールされた容器を含む。
下記の実施例は、本発明の好ましい態様を説明するために含まれている。以下の実施例で開示された技術は、本発明者によって発見された、本発明の実施に当たりうまく機能させるための技術を代表するものであると当業者に認識されるべきであり、したがって、その実施に当たり好ましい様式を構成すると考えられうる。しかし当業者は、本発明の開示に当たり、開示された特定の態様において多数の修正がなされえ、本発明の精神と範囲を逸脱しない類似の結果をなお得ることができると認識すべきである。
繊維状形態を伴う高表面積シリカナノ球体
本発明のナノ粒子の製造にはまず、シクロヘキサン:ペンタノール:水の混合物中に、テンプレートとしての臭化セチルピリジニウム(CPB)及び尿素を使用したミクロエマルジョンの形成が行われた。シリカ前駆体(オルト珪酸テトラエチル)は、分解した尿素によって加水分解され、その後、これらの加水分解され負に荷電した珪酸分子が、自己組織化したテンプレート(CPB)分子の間にできた空間に集まり(図1)、自由な放射状方向及び制限された接線方向に凝集した。最後に、自己組織化した珪酸の縮合によって、(溶媒中に分散した)個々のミセル内でのシリカ材料の結晶化がもたらされ、繊維状シリカナノ球体が生産された。
Claims (53)
- 複数の繊維を含むナノ粒子であって、それぞれの繊維が他の一つの繊維と接触しており、それぞれの繊維が、約1nm〜約5000nmの長さであり、かつ約1nm〜約50nmの太さである、ナノ粒子。
- ナノ粒子がシリカで構成されている、請求項1記載のナノ粒子。
- それぞれの繊維が、約1nm〜約250nmの長さである、請求項1記載のナノ粒子。
- それぞれの繊維が、約1nm〜約25nmの太さである、請求項1記載のナノ粒子。
- それぞれの繊維が、約1nm〜約10nmの太さである、請求項1記載のナノ粒子。
- それぞれの繊維が、約1nm〜約250nmの長さであり、かつ約1nm〜約10nmの太さである、請求項1記載のナノ粒子。
- 繊維が、さまざまな太さ及びさまざまな長さである、請求項1記載のナノ粒子。
- 繊維が、均一の太さ及び均一の長さである、請求項1記載のナノ粒子。
- 約103〜106本の繊維で構成されている、請求項1記載のナノ粒子。
- 少なくとも約104本の繊維で構成されている、請求項9記載のナノ粒子。
- 少なくとも約105本の繊維で構成されている、請求項10記載のナノ粒子。
- ナノ球体の中で実質的に放射状に配向している複数の繊維から構成されるナノ球体としてさらに規定される、請求項1記載のナノ粒子。
- それぞれの繊維が、約1nm〜約250nmの長さであり、かつ約1nm〜約10nmの太さである、請求項12記載のナノ粒子。
- 一つまたは複数の繊維に付着した、一種または複数種のリガンドをさらに含む、請求項1記載のナノ粒子。
- 一種または複数種のリガンドが、金属触媒分子、医薬または有機分子である、請求項14記載のナノ粒子。
- リガンドが、リンカーを介して、または単なる吸収もしくは吸着によって繊維に付着している、請求項15記載のナノ粒子。
- リンカーが、アルキル、水素化物、カルベン、カルビン、シクロペンタジエニル、アルコキシド、アミド、またはイミド基を含む、請求項16記載のナノ粒子。
- リンカーが、アルキル、水素化物、カルベン、カルビン、シクロペンタジエニル、アルコキシド、アミド、またはイミド基である、請求項17記載のナノ粒子。
- リガンドが金属触媒分子である、請求項15記載のナノ粒子。
- 金属触媒分子が、金属イオンまたは金属酸化物である、請求項18記載のナノ粒子。
- 金属触媒分子が、Au、Pt、Pd、Ag、Ni、Ru、Rh、Ir、Os、Co、Fe、及びCuからなる群より選択される金属である、請求項19記載のナノ粒子。
- 金属触媒分子が、Al2O3、TiO2、Fe2O3、CeO2、CuO、ZnO、SiO2、V2O5、MgO、La2O3、ZrO2、SnO2、MnO2、MoO3、Mo2O5及びゼオライトからなる群より選択される金属酸化物である、請求項19記載のナノ粒子。
- 最大直径が約50nm〜約5000nmである、請求項1記載のナノ粒子。
- 最大直径が約100nm〜約750nmである、請求項22記載のナノ粒子。
- 最大直径が約250nm〜約500nmである、請求項23記載のナノ粒子。
- 請求項1〜24のいずれか一項記載のナノ粒子を含む、組成物。
- 請求項1〜24のいずれか一項記載のナノ粒子を含む、複合体。
- 請求項19〜21のいずれか一項記載のナノ粒子を含む、触媒。
- 組成物を、請求項19〜21のいずれか一項記載のナノ粒子に接触させる工程を含む、触媒を組成物に送達する方法。
- 触媒が金属または金属酸化物である、請求項28記載の方法。
- 以下の工程を含む、請求項1記載のナノ粒子を生産するための方法:
(a) シリカ前駆体、テンプレート分子、及び溶媒を含む組成物を準備する工程であって、テンプレート分子が式:
の化合物であり、
式中、
nが、5〜25の数字であり、
R1が、
または
または
であり、
式中、
X-が、Cl、Br、I、またはFであり、かつ
R2〜R9がそれぞれ独立して、H、Cl、Br、I、OH、及びC1-C10アルキルからなる群より選択される、工程;
(b)(a)の組成物を、熱またはマイクロ波照射にさらす工程であって、シリカを含む粒子が組成物中で形成される、工程;
(c)加熱またはマイクロ波照射された(b)の組成物から、溶媒の一部または全部を取り除き、単離されたシリカテンプレート粒子を生産する工程;及び
(d)(c)の単離されたシリカテンプレート粒子をか焼し、シリカナノ粒子を生産する工程。 - テンプレート分子が、臭化セチルピリジニウム(CPB)である、請求項30記載の方法。
- テンプレート分子が、臭化ヘキサデシルトリメチルアンモニウムである、請求項30記載の方法。
- 溶媒が、シクロヘキサン、ペンタノール、及び水からなる群より選択される一つまたは複数の溶媒を含む、請求項30記載の方法。
- (a)の組成物が尿素をさらに含む、請求項30記載の方法。
- (a)の組成物が熱にさらされる、請求項30記載の方法。
- (a)の組成物がマイクロ波照射にさらされる、請求項30記載の方法。
- リガンドを、(d)のナノ粒子の表面に付着させる工程をさらに含む、請求項30記載の方法。
- リガンドが金属である、請求項37記載の方法。
- 金属が、Au、Pt、Pd、Ag、Ni、Ru、Rh、Ir、Os、Co、Fe、及びCuからなる群より選択される、請求項38記載の方法。
- リガンドが金属酸化物である、請求項37記載の方法。
- 金属酸化物が、Al2O3、TiO2、Fe2O3、CeO2、CuO、ZnO、SiO2、V2O5、MgO、La2O3、ZrO2、SnO2、MnO2、MoO3、Mo2O5及びゼオライトからなる群より選択される、請求項40記載の方法。
- 以下の工程を含む、リガンドに付着した複数の繊維を含むシリカナノ粒子を製造するための方法:
(a) 複数の繊維を含むシリカナノ粒子を得る工程であって、それぞれの繊維が他の一つの繊維と接触しており、それぞれの繊維が、長さが約1nm〜約5000nmであり、かつ太さが約1nm〜約50nmである、工程;及び
(b) リガンドを、ナノ粒子上の繊維に付着させる工程。 - リガンドが触媒である、請求項42記載の方法。
- 反応混合物を、請求項19〜21のいずれか一項記載のナノ粒子と接触させる工程を含む、反応混合物中で反応を触媒する方法。
- 一つまたは複数のシールされた容器中に、請求項1〜21のいずれか一項記載のナノ粒子を含む、キット。
- ナノ粒子が、クロマトグラフィーカラム中に含まれる、請求項45記載のキット。
- 請求項1〜21のいずれか一項記載のナノ粒子を含む固定相を含む、クロマトグラフィーカラム。
- 請求項1〜21のいずれか一項記載のナノ粒子を含む、医薬送達装置。
- 請求項1〜24のいずれか一項記載のナノ粒子を水または油に接触させる工程を含む、油または水から金属を取り除くための方法であって、該水または油が、金属を含むことが既知であるかまたは金属を含むことが疑われる、方法。
- 請求項1〜24のいずれか一項記載のナノ粒子を、エネルギー源に接触させる工程を含む、エネルギーを貯蔵するための方法。
- エネルギー源が水素である、請求項50記載の方法。
- 請求項1〜24のいずれか一項記載のナノ粒子を含む、包装材料。
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