JP2008528825A - セラミック中空繊維複合体、その生産方法およびその使用 - Google Patents
セラミック中空繊維複合体、その生産方法およびその使用 Download PDFInfo
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- JP2008528825A JP2008528825A JP2007553500A JP2007553500A JP2008528825A JP 2008528825 A JP2008528825 A JP 2008528825A JP 2007553500 A JP2007553500 A JP 2007553500A JP 2007553500 A JP2007553500 A JP 2007553500A JP 2008528825 A JP2008528825 A JP 2008528825A
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- Prior art keywords
- ceramic
- composite
- hollow
- oxygen
- hollow fiber
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
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- 239000012510 hollow fiber Substances 0.000 title claims abstract description 106
- 239000000919 ceramic Substances 0.000 title claims abstract description 69
- 239000002131 composite material Substances 0.000 title claims abstract description 62
- 238000004519 manufacturing process Methods 0.000 title claims description 32
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 65
- 239000001301 oxygen Substances 0.000 claims abstract description 61
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 46
- 229910010293 ceramic material Inorganic materials 0.000 claims abstract description 44
- 239000000203 mixture Substances 0.000 claims abstract description 42
- -1 oxygen anions Chemical class 0.000 claims abstract description 17
- 239000000463 material Substances 0.000 claims abstract description 16
- 238000005245 sintering Methods 0.000 claims abstract description 16
- 239000007789 gas Substances 0.000 claims abstract description 15
- 239000012530 fluid Substances 0.000 claims abstract description 12
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 11
- 239000000835 fiber Substances 0.000 claims description 34
- 150000001768 cations Chemical class 0.000 claims description 29
- 238000000034 method Methods 0.000 claims description 23
- 229920000642 polymer Polymers 0.000 claims description 21
- 239000011224 oxide ceramic Substances 0.000 claims description 16
- 229910052574 oxide ceramic Inorganic materials 0.000 claims description 16
- 239000012700 ceramic precursor Substances 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 8
- 229910052751 metal Inorganic materials 0.000 claims description 7
- 239000002184 metal Substances 0.000 claims description 7
- 150000002602 lanthanoids Chemical class 0.000 claims description 5
- 230000003647 oxidation Effects 0.000 claims description 5
- 229910052788 barium Inorganic materials 0.000 claims description 4
- 229910052742 iron Inorganic materials 0.000 claims description 4
- 229910052747 lanthanoid Inorganic materials 0.000 claims description 4
- 230000007704 transition Effects 0.000 claims description 4
- 150000002739 metals Chemical class 0.000 claims description 3
- 230000007935 neutral effect Effects 0.000 claims description 3
- 239000011148 porous material Substances 0.000 claims description 3
- 230000003197 catalytic effect Effects 0.000 claims description 2
- 238000000578 dry spinning Methods 0.000 claims description 2
- 238000002074 melt spinning Methods 0.000 claims description 2
- 150000002894 organic compounds Chemical class 0.000 claims description 2
- 230000000737 periodic effect Effects 0.000 claims description 2
- 239000002994 raw material Substances 0.000 claims description 2
- 229910052712 strontium Inorganic materials 0.000 claims description 2
- 238000002166 wet spinning Methods 0.000 claims description 2
- 229910052725 zinc Inorganic materials 0.000 claims description 2
- 229910052726 zirconium Inorganic materials 0.000 claims description 2
- 238000009940 knitting Methods 0.000 claims 2
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- 238000009941 weaving Methods 0.000 claims 1
- 238000007599 discharging Methods 0.000 abstract 1
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- 230000035699 permeability Effects 0.000 description 6
- 239000000853 adhesive Substances 0.000 description 4
- 230000001070 adhesive effect Effects 0.000 description 4
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 230000001747 exhibiting effect Effects 0.000 description 2
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- 239000007788 liquid Substances 0.000 description 2
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- 238000001556 precipitation Methods 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 description 1
- 206010021143 Hypoxia Diseases 0.000 description 1
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- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
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- 239000000654 additive Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- WUKWITHWXAAZEY-UHFFFAOYSA-L calcium difluoride Chemical compound [F-].[F-].[Ca+2] WUKWITHWXAAZEY-UHFFFAOYSA-L 0.000 description 1
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- 238000005520 cutting process Methods 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 239000010436 fluorite Substances 0.000 description 1
- 239000012784 inorganic fiber Substances 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
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- 150000002500 ions Chemical class 0.000 description 1
- 238000005304 joining Methods 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
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- 229920002647 polyamide Polymers 0.000 description 1
- 229920000412 polyarylene Polymers 0.000 description 1
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- 210000005239 tubule Anatomy 0.000 description 1
- 238000004804 winding Methods 0.000 description 1
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Abstract
他の複合体は、酸素輸送性セラミック材料であって、酸素アニオンおよび電子を伝導するセラミック材料であるか、または酸素アニオンを伝導するセラミック材料と電子を伝導するセラミックもしくは非セラミック材料との組合わせである前記酸素輸送性セラミック材料の中空繊維を少なくとも1つと、少なくとも一端面における流体の導入または放出のための接続要素とを含み、ここにおいて、中空繊維と接続要素は接合されている。
該複合体は、酸素含有ガス混合物から酸素を単離するため、または酸化反応を実施するために、用いることができる。
【選択図】 なし
Description
中空セラミック繊維は、それ自体が公知である。それらの生産については、例えば、US−A−4222977またはUS−A−5707584に記載されている。
第一に、セラミック材料で構成される膜は気密性に作成することができ、第二に、選択されたセラミック材料は酸素透過性を示し、したがって、ガス混合物から酸素を分離するのに用いることができる。そのようなセラミックスの考えうる用途は、とりわけ、ガス分離のような高温での用途または新規タイプの膜反応器である。
このようにして生産された繊維は、比較的高い機械的安定性を有するが、当然ながら、セラミック材料に特有の脆性および破壊に対する過敏性を示す。
本発明の他の目的は、これらの構造体の簡単な生産方法であって、セラミック造形体を生産するための通例の装置を用いることができる方法を提供することである。
本説明の目的に関し、中空繊維は、中空の内部空間を有し、あらゆる外部寸法、すなわち、直径または線寸法を有することができる構造体である。
中空繊維の好ましい外径または線寸法は、最大5mmの範囲で変動する。3mm未満の外径を有する中空繊維を用いることが、とりわけ好ましい。
例えば、以下の複合体を生産することが可能である:
・平面状に配置され縦方向に接触している複数の中空繊維
・複数の編組された中空繊維または複数の一緒に加撚された中空繊維
・モノリス(monolith)を形成するように組み合わされた複数の中空繊維(中空繊維で作られた多流路要素)。
紡糸する組成物中の可紡性ポリマーの含量は広い範囲内で変動することができるが、紡糸する組成物または紡糸液の全体に基づき通常2〜30重量%、好ましくは5〜10重量%である。
可紡性ポリマーおよび微細セラミック材料またはその前駆体のタイプおよび量は、可紡性ポリマーの含量をできるだけ低く保ちつつなお可紡性である組成物が得られるように選択することが好ましい。
造形に続く加工段階において、得られた未処理中空繊維を組み合わせて、所望の複合体を形成する。
本発明の複合体の酸素輸送に関する典型的な値は、当該複合体の全表面にわたる平均として測定して、少なくとも0.01標準cm3/(min*cm2)、好ましくは少なくとも0.1標準cm3/(min*cm2)の酸素流束である。ここで、標準cm3は、標準立方センチメートル(1barおよび25℃における)である。酸素流束に関して与えられる値は、本説明の目的の場合、950℃において2つの自由な気相(free gas phase)間の酸素分圧差0.2barで決定され、ここにおいて、高い方の酸素分圧が0.2barである。
i)ポリマーと、セラミック、とりわけ酸化物セラミック、またはセラミックの前駆体とを含む組成物を、ノズル、好ましくは環状ノズルに通して、それ自体が公知の方法で押し出すことによる、未処理中空繊維の生産、
ii)段階i)で生産された1以上の未処理中空繊維からの、該未処理中空繊維(1以上)の外表面(1以上)の間に接点を形成することによる、未処理複合体の生産、および
iii)ポリマーを除去し、段階i)でセラミックの前駆体を使用する場合はセラミックを形成し、中空セラミック繊維の間に接点を構築するための、段階ii)で生産された未処理複合体の熱処理、
を含む方法を提供する。
i)ポリマーと、セラミック、とりわけ酸化物セラミック、またはセラミックの前駆体とを含む組成物を、ノズル、好ましくは環状ノズルに通して、それ自体が公知の方法で押し出すことによる、未処理中空繊維の生産、
iv)段階i)で生産された1以上の未処理中空繊維と、該未処理中空繊維の少なくとも一端面において流体を導入または放出するための少なくとも1つの接続要素からの、未処理複合体の生産、および
v)ポリマーを除去し、中空セラミック繊維と少なくとも1つの接続要素の間に接点を構築し、そしてまた、段階i)でセラミックの前駆体を使用する場合はセラミック、とりわけ酸化物セラミックを形成するための、段階iv)で生産された未処理複合体の熱処理、
を含む方法を提供する。
繊維の横断面が非円形である場合、Deは外側横断面の最大寸法であり、Diは内側横断面の最大寸法である。
引取速度は、通常1分あたり1〜100m、好ましくは5〜20m/minである。
本発明はさらに、酸化反応の実施、とりわけ有機化合物の接触酸化のための、上記複合体の使用を規定する。
実施例1:未処理中空繊維の生産
組成BaCo0.4Fe0.4Zr0.2O3-δを有するセラミック粉末を、ポリスルホン(UDEL P−3500、Solvay)および1−メチル−2−ピロリドン(NMP)(≧99.0%、Merck)と一緒に撹拌して、スリップを生産した。その後、これをボールミルで均質化した。
実施例1に記載したように生産した複数の中空繊維を、それらがその外壁に沿って接触するように互いに平行に配置した。未処理中空繊維のこの複合体を、炉内に吊り下げて焼結した。
・96℃/h 500℃(1h保持)
・120℃/h 1000℃
・60℃/h 1300℃(6h保持)
・120℃/h 800℃
・180℃/h 80℃
焼結後、個々の中空繊維の凝集複合体が得られた。個々の中空繊維は、30〜35cmの長さ、ならびに0.8〜0.9mmのDe径および0.5〜0.6mmのDi径を有していた。
実施例3:中空セラミック繊維で構成される他の複合体の生産
実施例1に記載したように生産した複数の中空繊維を手で編組し、実施例2に記載した方法により熱的に処理した。
実施例3に記載したように生産した中空繊維は、酸素に対する選択的透過性を有していた。
実施例1に記載したように生産した複数の中空繊維を、それらが、管状多流路要素であって、該要素の個々の細管が互いに平行に延長している中空繊維である、前記管状多流路要素を形成するように、ロッド形の型の表面上で互いに手で組合わせた。
焼結し、ロッド形の型を取り外した後、多流路要素の内部空間は空であった。平行な中空繊維で構成される多流路要素であって、該中空繊維が一緒に焼結されていて酸素に対する選択的透過性を有する、前記多流路要素が得られた。
実施例1に記載したように生産した複数の中空繊維を、それらが、個々の細管がらせんに沿って互いに接触しているらせん形の多流路要素を形成するように、ロッド形の型の表面に沿って巻き付けた。
焼結し、ロッド形の型を取り外した後、多流路要素の内部空間は空であった。中空繊維で構成される多流路要素であって、該中空繊維が一緒に焼結されていて、らせん形に互いに平行に延長しており、酸素に対する選択的透過性を有する、前記多流路要素が得られた。
実施例1に記載したように生産した複数の中空繊維を、それらが、多流路要素であって、該要素の個々の細管が互いに平行に延長している中空繊維である、前記多流路要素を形成するように、互いに手で組合わせた。多流路要素の内部空間は、横断面で見ると、中空繊維で完全に満たされていた。
得られた未処理複合体を、実施例2に記載した方法により熱的に処理した。
ガスの導入および放出のための金属性接続要素を未処理多流路要素に付着させないという変更をして、実施例6を繰り返した。セラミック多流路要素の焼結後、2つの接続要素を、セラミック接着剤を用いてセラミック中空繊維の両端面で接合した。その後、この複合体を100℃で加熱して、両端面に金属性接続要素が付着している多流路要素を得た。
Claims (25)
- 酸素輸送性セラミック材料の中空繊維を少なくとも1つ含む複合体であって、該材料が、酸素アニオンおよび電子を伝導するセラミック材料であるか、または酸素アニオンを伝導するセラミック材料と電子を伝導するセラミックもしくは非セラミック材料との組合わせであり、該中空繊維の外表面が、同じ中空繊維または酸素輸送性セラミック材料の他の中空繊維の外表面と接触しており、該接触点が焼結により接合されている、前記複合体。
- 酸素輸送性セラミック材料の中空繊維を少なくとも1つ含む複合体であって、該材料が、酸素アニオンおよび電子を伝導するセラミック材料であるか、または酸素アニオンを伝導するセラミック材料と電子を伝導するセラミックもしくは非セラミック材料との組合わせであり、流体の導入または放出のための1つまたは2つの接続要素が、該中空繊維の少なくとも一端面、好ましくは両端面に提供されている、前記複合体。
- 一緒に編組または加撚されている複数の中空繊維を含むことを特徴とする、請求項1または2のいずれかに記載の複合体。
- 少なくとも2つの中空繊維を含むことを特徴とする請求項1または2のいずれかに記載の複合体であって、該中空繊維が、酸素輸送性セラミック材料で構成され、互いに平行に延長しており、それらの外壁がそれらの長さの少なくとも一部に沿って接触している、前記複合体。
- 複数の平行な中空繊維または管を含むことを特徴とする請求項4に記載の複合体であって、該中空繊維または管が管状多流路要素の形態で配置されており、それらの外壁がそれらの長さの少なくとも一部に沿って接触している、前記複合体。
- 中空繊維または管が管状多流路要素の外壁を形成し、該管状多流路要素の内部空間が、中空であるか、ロッド形の強化材料を含むことを特徴とする、請求項5に記載の複合体。
- 中空繊維または管が、気密性または多孔性材料で構成される管の内側に沿って平行に延長していることを特徴とする、請求項6に記載の複合体。
- 管状多流路要素の中空内部空間が酸化触媒を含むことを特徴とする、請求項6に記載の複合体。
- 互いに製織されているか、形成ループ編成されているか、または引き抜きループ編成されている1以上の中空繊維を含むことを特徴とする、請求項1または2のいずれかに記載の複合体。
- 酸素輸送性セラミック材料が酸化物セラミックであることを特徴とする、請求項1または2のいずれかに記載の複合体。
- 酸化物セラミックが、ペロブスカイト型構造またはブラウンミラライト型構造またはアウリビリウス型構造を有することを特徴とする、請求項10に記載の複合体。
- 酸化物セラミックがペロブスカイト型構造ABO3-δを有することを特徴とする請求項11に記載の複合体であって、Aが二価のカチオンであり、Bが三価以上のカチオンであり、Aのイオン半径がBのイオン半径より大きく、δが、材料が電気的に中性になるように、0.01〜0.9、好ましくは0.01〜0.5であり、そして、Aおよび/またはBが、異なるカチオンの混合物として存在することができる、前記複合体。
- 酸化物セラミックがブラウンミラライト型構造A2B2O5-δを有することを特徴とする請求項11に記載の複合体であって、Aが二価のカチオンであり、Bが三価以上のカチオンであり、Aのイオン半径がBのイオン半径より大きく、δが、材料が電気的に中性になるように、0.01〜0.9、好ましくは0.01〜0.5であり、そして、Aおよび/またはBが、異なるカチオンの混合物として存在することができる、前記複合体。
- タイプAのカチオンが、主族II、遷移族I、遷移族II、ランタニド族のカチオン、またはこれらのカチオンの混合物の中から、好ましくは、Mg2+、Ca2+、Sr2+、Ba2+、Cu2+、Ag2+、Zn2+、Cd2+および/またはランタニドの中から選択されることを特徴とする、請求項12または13に記載の複合体。
- タイプBのカチオンが、周期表のIIIB〜VIIIB族および/もしくはランタニド族、主族Vの金属のカチオン、またはこれらのカチオンの混合物の中から、好ましくは、Fe3+、Fe4+、Ti3+、Ti4+、Zr3+、Zr4+、Ce3+、Ce4+、Mn3+、Mn4+、Co2+、Co3+、Nd3+、Nd4+、Gd3+、Gd4+、Sm3+、Sm4+、Dy3+、Dy4+、Ga3+、Yb3+、Al3+、Bi4+、またはこれらのカチオンの混合物の中から選択されることを特徴とする、請求項12または13に記載の複合体。
- ペロブスカイト型構造を有する酸素輸送性酸化物セラミックが、元素Ba、Sr、Fe、ZnおよびOまたは元素Ba、Co、Fe、ZrおよびOを含む、好ましくは、組成物BaCoxFeyZrzO3-δ[式中、x、yおよびzの合計は1であり、zは0.1〜0.5の値をとり、xはa*yの範囲内の値を有し、aは0.8〜1.2の値をとり、δは請求項12で定義した意味を有する]を含むことを特徴とする、請求項12に記載の複合体。
- 請求項1に記載の複合体の生産方法であって、処置:
i)ポリマーと、セラミック、とりわけ酸化物セラミック、またはセラミックの前駆体とを含む組成物を、ノズル、好ましくは環状ノズルに通して、それ自体が公知の方法で押し出すことによる、未処理中空繊維の生産、
ii)段階i)で生産された1以上の未処理中空繊維からの、該未処理中空繊維(1以上)の外表面(1以上)の間に接点を形成することによる、未処理複合体の生産、および
iii)ポリマーを除去し、段階i)でセラミックの前駆体を使用する場合はセラミックを形成し、中空セラミック繊維の間に接点を構築するための、段階ii)で生産された未処理複合体の熱処理、
を含む前記方法。 - 押出を、乾式紡糸法、湿式紡糸法、または溶融紡糸法に従って実施することを特徴とする、請求項17に記載の方法。
- 複合体の生産を、未処理中空繊維(1以上)の編組、加撚、製織、形成ループ編成、引き抜きループ編成により、または未処理中空繊維を互いに平行に置くことにより、達成することを特徴とする、請求項17に記載の方法。
- 未処理中空繊維がロッド形の強化要素の周囲または管の周囲に配置されていることを特徴とする、請求項19に記載の方法。
- 段階ii)で生産された未処理複合体の熱処理を900〜1600℃の範囲の温度で実施することを特徴とする、請求項17に記載の方法。
- 段階iii)で生産された複合体を、流体の導入または放出のための少なくとも1つの接続要素に中空繊維の少なくとも一端面において接合する、好ましくは接着結合することを特徴とする、請求項17に記載の方法。
- 請求項2に記載した複合体の生産方法であって、処置:
i)ポリマーと、セラミック、とりわけ酸化物セラミック、またはセラミックの前駆体とを含む組成物を、ノズル、好ましくは環状ノズルに通して、それ自体が公知の方法で押し出すことによる、未処理中空繊維の生産、
iv)段階i)で生産された1以上の未処理中空繊維と、該未処理中空繊維の少なくとも一端面において流体を導入または放出するための少なくとも1つの接続要素からの、未処理複合体の生産、および
v)ポリマーを除去し、中空セラミック繊維と少なくとも1つの接続要素の間に接点を構築し、そしてまた、段階i)でセラミックの前駆体を使用する場合はセラミック、とりわけ酸化物セラミックを形成するための、段階iv)で生産された未処理複合体の熱処理、
を含む前記方法。 - 酸素含有ガス混合物、とりわけ空気から酸素を単離するための、請求項1〜16のいずれかに記載の複合体の使用。
- 酸化反応の実施、とりわけ有機化合物の接触酸化のための、請求項1〜16のいずれかに記載の複合体の使用。
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JP2012026066A (ja) * | 2010-07-28 | 2012-02-09 | Japan Atomic Energy Agency | セラミックスマイクロチューブの作製方法 |
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