JP7264048B2 - 金属酸化物繊維の製造方法 - Google Patents
金属酸化物繊維の製造方法 Download PDFInfo
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- JP7264048B2 JP7264048B2 JP2019516724A JP2019516724A JP7264048B2 JP 7264048 B2 JP7264048 B2 JP 7264048B2 JP 2019516724 A JP2019516724 A JP 2019516724A JP 2019516724 A JP2019516724 A JP 2019516724A JP 7264048 B2 JP7264048 B2 JP 7264048B2
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- polymetalloxane
- metal oxide
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- 239000002184 metal Substances 0.000 claims description 59
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- 229910052718 tin Inorganic materials 0.000 claims description 17
- 229920000620 organic polymer Polymers 0.000 claims description 12
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 11
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- 125000003118 aryl group Chemical group 0.000 claims description 9
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- KWGKDLIKAYFUFQ-UHFFFAOYSA-M lithium chloride Chemical compound [Li+].[Cl-] KWGKDLIKAYFUFQ-UHFFFAOYSA-M 0.000 description 8
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- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 2
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- JEGNMOIIQPASIC-UHFFFAOYSA-N dibutoxyalumanyloxy(trimethyl)silane Chemical compound CCCCO[Al](O[Si](C)(C)C)OCCCC JEGNMOIIQPASIC-UHFFFAOYSA-N 0.000 description 1
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- ROPILACPUDGYBZ-UHFFFAOYSA-N dipropoxyalumanyloxy(trimethyl)silane Chemical compound CCCO[Al](O[Si](C)(C)C)OCCC ROPILACPUDGYBZ-UHFFFAOYSA-N 0.000 description 1
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- GUVUOGQBMYCBQP-UHFFFAOYSA-N dmpu Chemical compound CN1CCCN(C)C1=O GUVUOGQBMYCBQP-UHFFFAOYSA-N 0.000 description 1
- 125000003438 dodecyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
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- 125000004051 hexyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
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- 230000003301 hydrolyzing effect Effects 0.000 description 1
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- XLSMFKSTNGKWQX-UHFFFAOYSA-N hydroxyacetone Chemical compound CC(=O)CO XLSMFKSTNGKWQX-UHFFFAOYSA-N 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- GJRQTCIYDGXPES-UHFFFAOYSA-N iso-butyl acetate Natural products CC(C)COC(C)=O GJRQTCIYDGXPES-UHFFFAOYSA-N 0.000 description 1
- FGKJLKRYENPLQH-UHFFFAOYSA-M isocaproate Chemical compound CC(C)CCC([O-])=O FGKJLKRYENPLQH-UHFFFAOYSA-M 0.000 description 1
- JMMWKPVZQRWMSS-UHFFFAOYSA-N isopropanol acetate Natural products CC(C)OC(C)=O JMMWKPVZQRWMSS-UHFFFAOYSA-N 0.000 description 1
- 229940011051 isopropyl acetate Drugs 0.000 description 1
- GWYFCOCPABKNJV-UHFFFAOYSA-N isovaleric acid Chemical compound CC(C)CC(O)=O GWYFCOCPABKNJV-UHFFFAOYSA-N 0.000 description 1
- OQAGVSWESNCJJT-UHFFFAOYSA-N isovaleric acid methyl ester Natural products COC(=O)CC(C)C OQAGVSWESNCJJT-UHFFFAOYSA-N 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 125000001624 naphthyl group Chemical group 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 125000002347 octyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 125000000962 organic group Chemical group 0.000 description 1
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- 125000001147 pentyl group Chemical group C(CCCC)* 0.000 description 1
- 125000000286 phenylethyl group Chemical group [H]C1=C([H])C([H])=C(C([H])=C1[H])C([H])([H])C([H])([H])* 0.000 description 1
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- 229910052697 platinum Inorganic materials 0.000 description 1
- 229920000233 poly(alkylene oxides) Polymers 0.000 description 1
- 229920000193 polymethacrylate Polymers 0.000 description 1
- 229920001296 polysiloxane Polymers 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 229920000036 polyvinylpyrrolidone Polymers 0.000 description 1
- 239000001267 polyvinylpyrrolidone Substances 0.000 description 1
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 description 1
- GNZVOBJWPAARFX-UHFFFAOYSA-N propan-2-olate;trimethylsilyloxyaluminum(2+) Chemical compound CC(C)[O-].CC(C)[O-].C[Si](C)(C)O[Al+2] GNZVOBJWPAARFX-UHFFFAOYSA-N 0.000 description 1
- LLHKCFNBLRBOGN-UHFFFAOYSA-N propylene glycol methyl ether acetate Chemical compound COCC(C)OC(C)=O LLHKCFNBLRBOGN-UHFFFAOYSA-N 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
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- 125000002914 sec-butyl group Chemical group [H]C([H])([H])C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000013076 target substance Substances 0.000 description 1
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 1
- VXYADVIJALMOEQ-UHFFFAOYSA-K tris(lactato)aluminium Chemical compound CC(O)C(=O)O[Al](OC(=O)C(C)O)OC(=O)C(C)O VXYADVIJALMOEQ-UHFFFAOYSA-K 0.000 description 1
- 125000002948 undecyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
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Classifications
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
- D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/04—Oxides; Hydroxides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G25/00—Compounds of zirconium
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G25/00—Compounds of zirconium
- C01G25/02—Oxides
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/62227—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products obtaining fibres
- C04B35/62231—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products obtaining fibres based on oxide ceramics
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/62227—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products obtaining fibres
- C04B35/62231—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products obtaining fibres based on oxide ceramics
- C04B35/62236—Fibres based on aluminium oxide
-
- C—CHEMISTRY; METALLURGY
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Description
本発明の実施の形態1に係る金属酸化物繊維の製造方法は、ポリメタロキサンおよび有機溶剤を含む組成物を紡糸して糸状物を得る紡糸工程と、この紡糸工程によって得られた糸状物を200℃以上2000℃以下の温度で焼成して、金属酸化物繊維を得る焼成工程と、を含む。この金属酸化物繊維の製造方法において、ポリメタロキサンは、Al、Sc、Ti、V、Cr、Mn、Fe、Co、Ni、Cu、Zn、Ga、Ge、Y、Zr、Nb、Mo、Pd、Ag、In、Sn、Sb、Hf、Ta、WおよびBiからなる群より選ばれる金属原子と酸素原子との繰り返し構造を有する。また、このポリメタロキサンの重量平均分子量は、2万以上200万以下である。以下、本発明におけるポリメタロキサンおよび有機溶剤は、各々、ポリメタロキサン(a)、有機溶剤(b)と適宜称する。
ポリメタロキサンとは、一般に、金属-酸素-金属結合を主鎖とする高分子である。本発明において、ポリメタロキサン(a)を構成する金属原子は、Al、Sc、Ti、V、Cr、Mn、Fe、Co、Ni、Cu、Zn、Ga、Ge、Y、Zr、Nb、Mo、Pd、Ag、In、Sn、Sb、Hf、Ta、WおよびBiからなる群より選ばれる。ポリメタロキサン(a)が上記金属原子を含むことにより、耐熱性の高い金属酸化物繊維を得ることができる。上記金属原子は、好ましくは、Al、Ti、ZrおよびSnからなる群より選ばれる金属原子である。詳細には、ポリメタロキサン(a)中の金属原子は、Al、Ti、ZrおよびSnからなる群より選ばれる金属原子を1種以上含むことが好ましい。ポリメタロキサン(a)が上記の好ましい金属原子を含むことにより、後述するポリメタロキサンの合成原料となる金属アルコキシドが安定に存在するため、高分子量のポリメタロキサンを得ることが容易となる。
本発明におけるポリメタロキサン(a)の合成方法は、特に制限はないが、下記一般式(3)で表される化合物および下記一般式(4)で表される化合物のうち少なくとも一つを、必要に応じて加水分解し、その後、部分縮合および重合させる縮重合工程を含むことが好ましい。
本発明の実施の形態1に係る金属酸化物繊維の製造方法に供される組成物は、上述したように、ポリメタロキサン(a)および有機溶剤(b)を含有する。この組成物は、有機溶剤(b)を含むことにより、任意の粘度に調節され得る。それにより、この組成物の曳糸性と流動性とを両立させることが可能となる。
本発明の実施の形態1に係る金属酸化物繊維の製造方法に供される組成物は、上述したポリメタロキサン(a)および有機溶剤(b)に加え、その他の成分を含んでいてもよい。その他の成分としては、界面活性剤、架橋剤、架橋促進剤などが挙げられる。
本発明の実施の形態1に係る金属酸化物繊維の製造方法は、上記組成物を紡糸して糸状物を得る紡糸工程と、この紡糸工程によって得られた糸状物を200℃以上2000℃以下の温度で焼成して、金属酸化物繊維を得る焼成工程とを含む。
紡糸工程において、組成物を紡糸する方法としては、公知の方法を用いることができる。例えば、この紡糸の方法として、乾式紡糸法、湿式紡糸法、乾湿式紡糸法、エレクトロスピニング法が挙げられる。
焼成工程では、上記紡糸工程で紡糸して得られた糸状物を200℃以上2000℃以下の温度で焼成し、これにより、架橋反応の進行とともに、有機基などの有機成分が除去され、強度に優れた金属酸化物繊維を得ることができる。この焼成工程における焼成の温度は、より好ましくは、400℃以上1500℃以下である。
(金属酸化物繊維)
本発明の実施の形態2に係る金属酸化物繊維は、以下に示す特徴的な構成を有する。すなわち、この実施の形態2に係る金属酸化物繊維は、Si(シリコン原子)と、Al、Sc、Ti、V、Cr、Mn、Fe、Co、Ni、Cu、Zn、Ga、Ge、Y、Zr、Nb、Mo、Pd、Ag、In、Sn、Sb、Hf、Ta、WおよびBiからなる群より選ばれる金属原子のうち1種以上と、を含む(以下、「第1の特徴」と適宜いう)。また、この金属酸化物繊維を構成する金属酸化物中のSiO2成分の含有量は、0.5重量%以下である(以下、「第2の特徴」と適宜いう)。
本発明に係る製造方法により得られる金属酸化物繊維は、連続した緻密な金属酸化物繊維であることから、高耐熱、高強度、表面活性などの特性を有する。そのため、当該金属酸化物繊維は、高耐熱繊維の特性を活かして、電気炉や建材などの断熱材や、放熱材として用いることができる。また、当該金属酸化物繊維は、高強度繊維の特性を活かして、繊維強化(FRP)などの複合材料として利用することができる。さらに、当該金属酸化物繊維は、高耐熱・高強度繊維の特性を活かして、航空機のエンジンタービンなどの部材や、宇宙航空機の部材として用いることができる。また、二酸化チタン主体の金属酸化物繊維によれば、光触媒活性を有するため、水および大気の浄化用フィルターなどに用いることができる。
合成例1のポリメタロキサン(T-1)溶液の合成方法について説明する。この合成方法では、トリイソプロポキシ(トリメチルシロキシ)チタン(31.4g(0.10mol))と、溶媒としてのNMP(15.8g)とを混合し、これを溶液1とした。また、水(5.4g(0.30mol))と、水希釈溶媒としてのイソプロピルアルコール(50.0g)と、重合触媒としてのトリブチルアミン(1.9g(0.01mol))とを混合し、これを溶液2とした。以下、イソプロピルアルコールは、IPAと略記する。
合成例2のポリメタロキサン(T-2)溶液の合成方法について説明する。この合成方法では、合成例1の溶媒であるNMP(15.8g)に替えて、γ-ブチロラクトン(15.8g)を溶媒として混合したこと以外は、合成例1と同様に合成を行った。以下、γ-ブチロラクトンは、GBLと略記する。
合成例3のポリメタロキサン(T-3)溶液の合成方法について説明する。この合成方法では、合成例1の重合触媒であるトリブチルアミン(1.9g)に替えて、ジシクロヘキシルメチルアミン(2.0g(0.01mol))を重合触媒として混合したこと以外は、合成例1と同様に合成を行った。
合成例4のポリメタロキサン(T-4)溶液の合成方法について説明する。この合成方法では、トリイソプロポキシ(トリメチルシロキシ)チタン(15.7g(0.05mol))と、テトラブトキシチタン(17.0g(0.05mol))と、溶媒としてのNMP(16.4g)とを混合し、これを溶液1とした。また、水(5.4g(0.30mol))と、水希釈溶媒としてのIPA(50.0g)と、重合触媒としてのトリブチルアミン(1.9g(0.01mol))とを混合し、これを溶液2とした。
合成例5のポリメタロキサン(Z-1)溶液の合成方法について説明する。この合成方法では、トリプロポキシ(トリメチルシロキシ)ジルコニウム(35.4g(0.10mol))と、溶媒としてのNMP(17.5g)とを混合し、これを溶液1とした。また、水(5.4g(0.30mol))と、水希釈溶媒としてのIPA(50.0g)と、重合触媒としてのトリブチルアミン(1.9g(0.01mol))とを混合し、これを溶液2とした。
合成例6のポリメタロキサン(A-1)溶液の合成方法について説明する。この合成方法では、ジ-s-ブトキシ(トリメチルシロキシ)アルミニウム(24.6g(0.10mol))と、溶媒としてのNMP(12.1g)とを混合し、これを溶液1とした。また、水(5.4g(0.30mol))と、水希釈溶媒としてのIPA(50.0g)と、重合触媒としてのトリブチルアミン(1.9g(0.01mol))とを混合し、これを溶液2とした。
合成例7のポリメタロキサン(TZ-1)溶液の合成方法について説明する。この合成方法では、トリイソプロポキシ(トリメチルシロキシ)チタン(15.7g(0.05mol))と、トリプロポキシ(トリメチルシロキシ)ジルコニウム(17.7g(0.05mol))と、溶媒としてのNMP(16.6g)とを混合し、これを溶液1とした。また、水(5.4g(0.30mol))と、水希釈溶媒としてのIPA(50.0g)と、重合触媒としてのトリブチルアミン(1.9g(0.01mol))とを混合し、これを溶液2とした。
合成例8のポリメタロキサン(TA-1)溶液の合成方法について説明する。この合成方法では、トリイソプロポキシ(トリメチルシロキシ)チタン(15.7g(0.05mol))と、ジ-s-ブトキシ(トリメチルシロキシ)アルミニウム(12.3g(0.05mol))と、溶媒としてのNMP(16.6g)とを混合し、これを溶液1とした。また、水(5.4g(0.30mol))と、水希釈溶媒としてのIPA(50.0g)と、重合触媒としてのトリブチルアミン(1.9g(0.01mol))とを混合し、これを溶液2とした。
合成例9のポリメタロキサン(ZA-1)溶液の合成方法について説明する。この合成方法では、トリプロポキシ(トリメチルシロキシ)ジルコニウム(17.7g(0.05mol))と、ジ-s-ブトキシ(トリメチルシロキシ)アルミニウム(12.3g(0.05mol))と、溶媒としてのNMP(16.6g)とを混合し、これを溶液1とした。また、水(5.4g(0.30mol))と、水希釈溶媒としてのIPA(50.0g)と、重合触媒としてのトリブチルアミン(1.9g(0.01mol))とを混合し、これを溶液2とした。
実施例1では、ポリメタロキサン(T-1)溶液(8.75g)にNMP(1.25g)を加え、固形分濃度を40.0%とし、組成物とした。この組成物の粘度は、2000Pであった。
実施例2~11では、表2に示した組成物につき、実施例1と同様に、糸状物を得た。次いで、表2に示した焼成温度で、実施例1と同様に糸状物を焼成し、金属酸化物繊維を得た。
比較例1では、ポリメタロキサンとしてB-10(商品名、日本曹達社製、ブトキシチタンオリゴマー、重量平均分子量2200)を用い、このB-10(4.00g)にNMP(6.0g)を加え、固形分濃度を40.0%とし、組成物とした。この組成物の粘度は、0.1Pであった。比較例1では、実施例1と同様にニードルから組成物を押し出したが、液滴となり、糸状物は得られなかった。
比較例2では、ポリメタロキサンとしてB-10に有機溶剤を加えずに、固形分濃度が100.0%の組成物とした。この組成物の粘度は、20Pであった。比較例2では、実施例1と同様にニードルから組成物を押し出したが、液滴となり、糸状物は得られなかった。
実施例12では、上述した実施例1で作製した金属酸化物繊維につき、元素組成をX線光電子分光法(以下、XPSと略す)により定量化した。XPSによる元素組成分析は、以下の方法で行った。具体的には、X線光電子分光装置(PHI社製、Quantera SXM)を用いて、試料に励起X線(monochromatic Al Kα1,2線(1486.6eV))を、X線径を200μmに設定して照射し、光電子脱出角度を45°とし、表面から放出される光電子をアナライザーで検出した。検出した光電子スペクトルのピーク位置およびピーク形状、ピーク面積比により、元素組成を定量した。
実施例13~22では、表2に示したように、実施例2~11で作製した金属酸化物繊維につき、実施例12と同様に、XPSによる元素組成分析およびXRDによる構造分析を行った。実施例13~22の分析結果は、表3に示した。
Claims (10)
- ポリメタロキサンおよび有機溶剤を含む組成物を紡糸して糸状物を得る紡糸工程と、
前記紡糸工程によって得られた前記糸状物を200℃以上2000℃以下の温度で焼成して、金属酸化物繊維を得る焼成工程と、
を含み、
前記ポリメタロキサンは、Al、Sc、Ti、V、Cr、Mn、Fe、Co、Ni、Cu、Zn、Ga、Ge、Y、Zr、Nb、Mo、Pd、Ag、In、Sn、Sb、Hf、Ta、WおよびBiからなる群より選ばれる金属原子と酸素原子との繰り返し構造を有し、
前記ポリメタロキサンの重量平均分子量は、2万以上200万以下であり、
前記ポリメタロキサンは、下記一般式(1)で表される構造単位および下記一般式(2)で表される構造単位のうち、下記一般式(2)で表される構造単位を少なくとも有するポリメタロキサンである、
ことを特徴とする金属酸化物繊維の製造方法。
- 前記組成物の25℃における粘度が10P以上50000P以下である、
ことを特徴とする請求項1に記載の金属酸化物繊維の製造方法。 - 平均繊維径が0.01μm以上1000μm以下である、
ことを特徴とする請求項1または2に記載の金属酸化物繊維の製造方法。 - 前記組成物が、有機高分子を含み、
前記組成物中の前記有機高分子の含有量が、前記組成物中に含まれる前記ポリメタロキサンの重量に対し、1重量%以下である、
ことを特徴とする請求項1~3のいずれか一つに記載の金属酸化物繊維の製造方法。 - 前記組成物が、アルカリ金属およびアルカリ土類金属をいずれも含まない、
ことを特徴とする請求項1~4のいずれか一つに記載の金属酸化物繊維の製造方法。 - 前記組成物が、珪酸、珪酸塩、シリカゲル、珪酸エステル、ホウ酸、ホウ酸塩およびホウ酸エステルをいずれも含まない、
ことを特徴とする請求項1~5のいずれか一つに記載の金属酸化物繊維の製造方法。 - 前記ポリメタロキサン中の前記金属原子Mが、Al、Ti、ZrおよびSnからなる群より選ばれる金属原子を1種以上含む、
ことを特徴とする請求項1~6のいずれか一つに記載の金属酸化物繊維の製造方法。 - 前記ポリメタロキサン中の前記金属原子Mは、Tiを含み、
前記金属酸化物繊維中の全ての前記金属原子MにおけるTiの比率が、5mol%以上100mol%以下の範囲である、
ことを特徴とする請求項1~7のいずれか一つに記載の金属酸化物繊維の製造方法。 - 前記ポリメタロキサン中の前記金属原子Mは、Zrを含み、
前記金属酸化物繊維中の全ての前記金属原子MにおけるZrの比率が、5mol%以上100mol%以下の範囲である、
ことを特徴とする請求項1~7のいずれか一つに記載の金属酸化物繊維の製造方法。 - 前記紡糸工程が、乾式紡糸法またはエレクトロスピニング法によって前記組成物を紡糸する工程である、
ことを特徴とする請求項1~9のいずれか一つに記載の金属酸化物繊維の製造方法。
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WO2014045527A1 (ja) | 2012-09-18 | 2014-03-27 | ニチアス株式会社 | 耐熱性を有する生体溶解性無機繊維及びその組成物 |
WO2014049988A1 (ja) | 2012-09-27 | 2014-04-03 | ニチアス株式会社 | 生体溶解性無機繊維及びその組成物 |
WO2017090512A1 (ja) | 2015-11-26 | 2017-06-01 | 東レ株式会社 | ポリメタロキサン、その製造方法、その組成物、硬化膜およびその製造方法ならびにそれを備えた部材および電子部品 |
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WO2019188834A1 (ja) | 2019-10-03 |
KR20200138205A (ko) | 2020-12-09 |
CN111886280A (zh) | 2020-11-03 |
CN111886280B (zh) | 2022-04-26 |
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JPWO2019188835A1 (ja) | 2021-03-11 |
US20210108339A1 (en) | 2021-04-15 |
SG11202009303SA (en) | 2020-10-29 |
US20210371599A1 (en) | 2021-12-02 |
KR20200138206A (ko) | 2020-12-09 |
TW201942211A (zh) | 2019-11-01 |
CN111971425A (zh) | 2020-11-20 |
JP7334619B2 (ja) | 2023-08-29 |
EP3778715B1 (en) | 2022-05-25 |
EP3778715A1 (en) | 2021-02-17 |
WO2019188835A1 (ja) | 2019-10-03 |
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