JP2022519076A - 複合材料及びその調製方法 - Google Patents
複合材料及びその調製方法 Download PDFInfo
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- JP2022519076A JP2022519076A JP2021544590A JP2021544590A JP2022519076A JP 2022519076 A JP2022519076 A JP 2022519076A JP 2021544590 A JP2021544590 A JP 2021544590A JP 2021544590 A JP2021544590 A JP 2021544590A JP 2022519076 A JP2022519076 A JP 2022519076A
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- 238000000034 method Methods 0.000 claims abstract description 38
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- 150000002739 metals Chemical class 0.000 claims abstract description 4
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- 239000000377 silicon dioxide Substances 0.000 claims description 62
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- 229910052760 oxygen Inorganic materials 0.000 claims description 53
- 239000000243 solution Substances 0.000 claims description 37
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- -1 silane compound Chemical class 0.000 claims description 20
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- DLOSDQIBVXBWTB-UHFFFAOYSA-N 1-[dimethyl(propyl)silyl]oxyethanamine Chemical compound CCC[Si](C)(C)OC(C)N DLOSDQIBVXBWTB-UHFFFAOYSA-N 0.000 description 1
- BHWUCEATHBXPOV-UHFFFAOYSA-N 2-triethoxysilylethanamine Chemical compound CCO[Si](CCN)(OCC)OCC BHWUCEATHBXPOV-UHFFFAOYSA-N 0.000 description 1
- QHQNYHZHLAAHRW-UHFFFAOYSA-N 2-trimethoxysilylethanamine Chemical compound CO[Si](OC)(OC)CCN QHQNYHZHLAAHRW-UHFFFAOYSA-N 0.000 description 1
- UNKZGKRGTGCFKH-UHFFFAOYSA-N 2-tripropoxysilylethanamine Chemical compound CCCO[Si](CCN)(OCCC)OCCC UNKZGKRGTGCFKH-UHFFFAOYSA-N 0.000 description 1
- VFYAYGBOSWNMGA-UHFFFAOYSA-N 3-[bis(trimethylsilyloxy)methylsilyl]propan-1-amine Chemical compound C[Si](C)(C)OC(O[Si](C)(C)C)[SiH2]CCCN VFYAYGBOSWNMGA-UHFFFAOYSA-N 0.000 description 1
- LAYIREOMKATBAT-UHFFFAOYSA-N 3-[dibutoxy(methyl)silyl]propan-1-amine Chemical compound CCCCO[Si](C)(CCCN)OCCCC LAYIREOMKATBAT-UHFFFAOYSA-N 0.000 description 1
- ZYAASQNKCWTPKI-UHFFFAOYSA-N 3-[dimethoxy(methyl)silyl]propan-1-amine Chemical compound CO[Si](C)(OC)CCCN ZYAASQNKCWTPKI-UHFFFAOYSA-N 0.000 description 1
- ZCSHOZYCEVDECE-UHFFFAOYSA-N 3-[dimethyl(propoxy)silyl]propan-1-amine Chemical compound CCCO[Si](C)(C)CCCN ZCSHOZYCEVDECE-UHFFFAOYSA-N 0.000 description 1
- FSMHYZUFHYGNHS-UHFFFAOYSA-N 3-[ethoxy-di(propan-2-yl)silyl]propan-1-amine Chemical compound CCO[Si](C(C)C)(C(C)C)CCCN FSMHYZUFHYGNHS-UHFFFAOYSA-N 0.000 description 1
- MCLXOMWIZZCOCA-UHFFFAOYSA-N 3-[methoxy(dimethyl)silyl]propan-1-amine Chemical compound CO[Si](C)(C)CCCN MCLXOMWIZZCOCA-UHFFFAOYSA-N 0.000 description 1
- XUZVALKTSQQLCH-UHFFFAOYSA-N 3-tripropoxysilylpropan-1-amine Chemical compound CCCO[Si](CCCN)(OCCC)OCCC XUZVALKTSQQLCH-UHFFFAOYSA-N 0.000 description 1
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- ZAPJNKRVHMYDOC-UHFFFAOYSA-N COC(OC)(OC)CO[SiH2]CCCN Chemical compound COC(OC)(OC)CO[SiH2]CCCN ZAPJNKRVHMYDOC-UHFFFAOYSA-N 0.000 description 1
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- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 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
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/103—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate comprising silica
-
- 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
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/02—Making microcapsules or microballoons
- B01J13/04—Making microcapsules or microballoons by physical processes, e.g. drying, spraying
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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
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
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Abstract
Description
本出願は、2019年1月31日に提出されたシンガポール出願番号10201900921Sに優先権があると主張するものであり、その開示内容は参考までに盛り込まれている。
本発明は、複合材料、その製造方法、複合材料の使用、及び酸素捕捉膜又は酸素バリア膜の形成方法に関する。
有利には、アニーリング又はエッチングプロセスによって、多孔質シリカ粒子は複合材料中により多くの金属粒子を保持するための、より大きな細孔/チャネルを有する。
本明細書で使用される以下の単語及び用語は、以下に示される意味を有するものとする:
エタノールと水との混合物中の金属/シリカ粒子の質量含有量は、約5重量%~約80重量%、約5重量%~約70重量%、約5重量%~約60重量%、約5重量%~約50重量%、約5重量%~約40重量%、約5重量%~約30重量%、約5重量%~約20重量%、約5重量%~約10重量%、約10重量%~約80重量%、約20重量%~約80重量%、約30重量%~約80重量%、約30重量%~約80重量%、約40重量%~約80重量%、約50重量%~約80重量%、約60重量%~約80重量%、又は約70重量%~約80重量%の範囲であってもよい。エタノールと水との混合物中の金属/シリカ粒子の質量含有量は、好ましくは約7~約10重量%の範囲であり得る。
添付の図面は開示された実施形態を示し、開示された実施形態の原理を説明するのに役立つ。しかしながら、図面は例示のみを目的として設計されたものであり、本発明の限定の定義として設計されたものではないことを理解されたい。
[図1]は、本明細書で定義される複合材料を形成するプロセス2を示す模式図である。
[図2]は、ポリマーコーティングを有する又は有しない、鉄/シリカナノ粒子の数個の透過型電子顕微鏡(TEM)画像を示す。図2(a)は、ポリマーコーティングを有しない鉄/シリカナノ粒子のTEM画像である。図2(b)は、0.1重量%EVOH溶液を用いて調製した、エチレンビニルアルコール共重合体(EVOH)被覆鉄/シリカナノ粒子のTEM画像である。図2(c)は、0.15重量%EVOH溶液を用いて調製した、EVOH被覆鉄/シリカナノ粒子のTEM画像である。図2(d)は、0.3重量%EVOH溶液を用いて調製した、EVOH被覆鉄/シリカナノ粒子のTEM画像である。
[図3]は、圧縮EVOHペレットの数個の光学画像を示す。図3(a)は、5重量%の鉄/シリカナノ粒子から作製された、圧縮EVOHペレットの光学画像である。ここに挿入されているのは、対応する圧縮EVOHペレットの写真である。図3(b)は、5重量%のEVOH被覆鉄/シリカナノ粒子から作製された、圧縮EVOHペレットの光学画像である。ここに挿入されているのは、対応する圧縮EVOHペレットの写真である。
図1に示すように、多孔質シリカ粒子200、シリカ粒子200の細孔100内に配置された複数の金属粒子300、及びシリカ粒子200を少なくとも部分的に封入するポリマーコーティング400を含む、複合材料500を形成するプロセス2が、提供される。最初に、細孔100を有するシリカ粒子200が提供され、次いで、金属粒子300が細孔100内に配置されることを可能にするために、細孔100のサイズを増加させるための、細孔拡大工程4に供される。細孔100のサイズが増加するにつれて、より多くの金属粒子300がシリカ粒子200内に存在することができる。次いで、これをポリマーコーティング工程6に供し、それによって金属/シリカ粒子は、ポリマー溶液に添加され、これが金属/シリカ粒子上にポリマーコーティング400を形成し、結果物である複合材料500を形成する。
臭化セチルトリメチルアンモニウム(CTAB)、塩化鉄(FeCl3)、塩化ナトリウム(NaCl)、エチレンビニルアルコール共重合体(EVOH)、アミノプロピルトリエトキシシラン(APTES)、テトラエチルオルトシリケート(TEOS)、エタノール、エチルエステル、及び水素化ホウ素ナトリウムを、Sigma Aldrich Singaporeから購入した。アンモニア(30%)を、Honey well Singaporeから購入した。水酸化ナトリウム(NaOH)を、Merck Singaporeから購入した。
0.6gのCTABを70mLの水に溶解し、0.6mLのアンモニア溶液(30%)及び20mLのエチルエステルと混合した。得られた溶液を、500rpm、30℃で30分間撹拌した。激しく撹拌しながら、3.5mLのTEOSを10分で溶液に滴下して加えた。TEOSの添加後、混合物を30℃で12時間撹拌した。得られたメソポーラスシリカナノ粒子を、9000rpmで10分間の遠心分離によって精製し、エタノールで2回洗浄した。シリカナノ粒子を、1M塩酸を含むエタノール溶液中に再分散させた。この懸濁液を500rpmで60℃で5時間撹拌し、次いで9000rpmで10分間遠心分離することによって精製して、シリカ粒子中の過剰なCTAB分子を除去した。CTABを除去する工程を繰り返して、CTABの大部分がシリカナノ粒子から確実に除去されるようにした。粒子を風乾し、次いで室温で真空乾燥した。
0.1重量%のNaOHによってエッチングされ、10重量%のAPTESで処理されたメソポーラスシリカを調製するために、実施例1の工程に従って多孔質シリカナノ粒子を調製した。1gの多孔質シリカナノ粒子を、500mlのエタノールに分散させた。10mLの水酸化ナトリウム(NaOH)溶液(0.1重量%)を懸濁液に加え、室温で3時間撹拌した。遠心分離によって精製した後、多孔質シリカナノ粒子を、0.1gのAPTESを含むエタノール溶液中に再分散させた。混合物を室温で1時間撹拌し続け、次いでナノ粒子を遠心分離によって収集した。
EVOHペレットを、体積比7:3のイソプロパノールと水との混合物に、65℃で溶解した。EVOH溶液100mLを試薬ボトルに入れ、65℃で撹拌し、窒素ガスで20分間バブリングして、溶液中の残留酸素を完全に除去した。塩化ナトリウム水溶液を、鉄/シリカナノ粒子の10重量%の質量含有量を有する鉄/シリカエタノール/水混合物に添加した。次に、0.5gの鉄/シリカナノ粒子を含む50mLのエタノール/水溶液を、EVOH溶液に滴下して加えた。懸濁液を室温に冷却し、窒素でバブリングした。窒素で10分間バブリングした水20mLを懸濁液に滴下した。EVOH被覆鉄/シリカナノ粒子を遠心分離によって精製し、真空オーブン中50℃で乾燥させた。(a)鉄/シリカナノ粒子、及び(b)0.1重量%、(c)0.15重量%及び(d)0.3重量%のEVOHを含むEVOH溶液を用いて調製したエチレンビニルアルコール共重合体(EVOH)被覆鉄/シリカナノ粒子のTEM像を図2に示す。図2(b)に示すように、エチレンビニルアルコール共重合体(EVOH)被覆は、観察されなかった。図2(c)に示すように、EVOHポリマー層の厚さは5nmであった。図2(d)に示すように、EVOHポリマー層の厚さは10nmであった。
EVOH被覆鉄/シリカナノ粒子の酸素捕捉性能を評価するために、実施例3から得られた各試料0.1gを25mlのガラス製円錐フラスコに入れた。フラスコ内に1mlの水を入れたガラス瓶を入れ、室内湿度(RH)を100%に調整した。次いで、フラスコを気密ゴム隔壁ストッパで密封し、酸素捕捉実験の間、室温に置いた。EVOH被覆鉄/シリカナノ粒子の酸素捕捉性能を表2に列挙する。0.1重量%のEVOHを含む鉄/シリカサンプルのポリマーコーティング厚さは、約1nmであった。0.15%EVOHを含む試料のポリマーコーティングの厚さは約5nmであり、0.3%EVOHを含む試料のポリマーコーティングの厚さは約10nmであった。参考までに、(ポリマーコーティング無し)鉄/シリカナノ粒子は、193.1cc/g Feの捕捉能力を示した。0.15重量%のEVOHを含むEVOH溶液によって調製されたEVOH被覆鉄/シリカナノ粒子は、より高い酸素捕捉能力(211cc/g Fe)を与えた。
鉄/シリカナノ粒子及びEVOH被覆鉄/シリカナノ粒子(0.15重量%のEVOH溶液を用いて調製)を、EVOHペレットと混合し、二軸スクリュー押出機を通して配合し、窒素ガスでフラッシュした。鉄/シリカナノ粒子及びEVOH被覆鉄/シリカナノ粒子の質量含有量を、5重量%に保った。得られたポリマーペレットをホットプレスにより圧縮して、薄膜を形成した。図2に示すように、EVOH被覆鉄/シリカを有する試料では、ナノ粒子の凝集がはるかに少なく観察され、その結果、より透明な膜が得られた。さらに、EVOH被覆鉄/シリカを有するEVOHペレットは、鉄/シリカ(0.52cc/gペレット)と配合した試料よりも高い酸素捕捉能力(1.14cc/gペレット)を有していた。(a)5重量%の鉄/シリカナノ粒子及び(b)5重量%のEVOH被覆鉄/シリカナノ粒子を含む圧縮EVOHペレットの光学画像及び対応する圧縮EVOHペレットの写真を図3に示す。光学画像に示すように、EVOH被覆鉄/シリカナノ粒子を含む試料では、鉄/シリカナノ粒子の凝集がはるかに少なく観察され、挿入図に示すように、より透明な膜が得られた。図3aの挿入図に示された膜は、140μmの厚さを有していた。図3aの挿入図に示された膜は、70μmの厚さを有していた。
Claims (26)
- 多孔質シリカ粒子、前記シリカ粒子の細孔内に配置された複数の金属粒子、及び前記シリカ粒子を少なくとも部分的に封入するポリマーコーティングを含む、複合材料。
- 前記シリカ粒子は、シラン化合物で修飾されている、請求項1に記載の複合材料。
- 前記シラン化合物は、アミノ基又はカルボン酸基で官能化されている、請求項2に記載の複合材料。
- 前記金属粒子の金属は、周期表の第8族から選択される、請求項1~3のいずれか一項に記載の複合材料。
- 前記金属粒子の金属は、鉄である、請求項1~4のいずれか一項に記載の複合材料。
- 前記金属粒子のサイズは、100nm未満である、請求項1~5のいずれか一項に記載の複合材料。
- 前記多孔質シリカ粒子のサイズは、20nm~1μmの範囲である、請求項1~6のいずれか一項に記載の複合材料。
- 前記多孔質シリカ粒子の細孔サイズは、5~50nmの範囲である、請求項1~7のいずれか一項に記載の複合材料。
- 前記複合材料中の金属粒子の重量は、前記多孔質シリカ粒子の乾燥重量に対して1~80重量%の範囲である、請求項1~8のいずれか一項に記載の複合材料。
- 活性化剤を更に含む、請求項1~9のいずれか一項に記載の複合材料。
- 前記活性化剤は、ハロゲン化物塩である、請求項10に記載の複合材料。
- 前記ポリマーコーティングは、ウレタン、アクリレート、メタクリレート、エポキシ、エチレン、ビニルアルコール及びそれらの混合物からなる群から選択されるモノマーを有するポリマーを含む、請求項1~11のいずれか一項に記載の複合材料。
- 前記ポリマーコーティングの厚さは、0.5~15nmの範囲である請求項1~12のいずれか一項に記載の複合材料。
- 前記複合材料は、210~230cm3/gの酸素捕捉性能を有することを特徴とする、請求項1~13のいずれか一項に記載の複合材料。
- 複合材料を調製する方法であって、複数の活性化金属及びシリカ粒子を含有する溶液をポリマー溶液と混合して、それによって前記複合材料を形成する工程を含み、前記複合材料は、多孔質シリカ粒子、前記シリカ粒子の細孔内に配置された複数の金属粒子、及び前記シリカ粒子を少なくとも部分的に封入するポリマーコーティングを含む、方法。
- 前記シリカ粒子の細孔サイズを拡大するために、アニール又は化学エッチングする工程を更に含む、請求項15に記載の方法。
- 前記アニール工程は、100~700℃で行われる、請求項16に記載の方法。
- 前記化学エッチング工程は、アルカリ塩溶液の使用を含む、請求項16に記載の方法。
- 前記溶液中のアルカリ塩の量が、シリカ粒子の0.01重量%~5重量%の範囲である、請求項18に記載の方法。
- シリカ粒子をシラン化合物で修飾する工程を更に含む、請求項15~19のいずれか一項に記載の方法。
- シラン化合物は、アミノ基又はカルボン酸基で官能化されている、請求項20に記載の方法。
- 前記ポリマー溶液の前記ポリマーが、アルコールと水との混合物に溶解される、請求項15~21のいずれか一項に記載の方法。
- 前記ポリマー溶液中の前記ポリマーの濃度は、0.01~10重量%の範囲である、請求項15~22のいずれか一項に記載の方法。
- 金属粒子を塩で活性化して前記活性化金属を形成する工程を更に含む、請求項15~23のいずれか一項に記載の方法。
- 請求項1~14のいずれか一項に記載の複合材料の、酸素捕捉材料としての使用。
- 請求項1~14のいずれか一項に記載の複合材料で、基材を配合又は被膜する工程を含む、酸素捕捉膜又は酸素バリア膜を形成する方法。
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