JP7056668B2 - エアロゲル及びその製造方法 - Google Patents
エアロゲル及びその製造方法 Download PDFInfo
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- JP7056668B2 JP7056668B2 JP2019546469A JP2019546469A JP7056668B2 JP 7056668 B2 JP7056668 B2 JP 7056668B2 JP 2019546469 A JP2019546469 A JP 2019546469A JP 2019546469 A JP2019546469 A JP 2019546469A JP 7056668 B2 JP7056668 B2 JP 7056668B2
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- Prior art keywords
- airgel
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- silane oligomer
- sol
- Prior art date
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- 238000004519 manufacturing process Methods 0.000 title claims description 25
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 88
- 229910000077 silane Inorganic materials 0.000 claims description 88
- 239000011240 wet gel Substances 0.000 claims description 73
- 238000001035 drying Methods 0.000 claims description 63
- 125000003545 alkoxy group Chemical group 0.000 claims description 23
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical group [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 21
- 239000003054 catalyst Substances 0.000 claims description 19
- 238000006460 hydrolysis reaction Methods 0.000 claims description 17
- 230000007062 hydrolysis Effects 0.000 claims description 15
- 239000003377 acid catalyst Substances 0.000 claims description 14
- 125000004430 oxygen atom Chemical group O* 0.000 claims description 11
- 230000003301 hydrolyzing effect Effects 0.000 claims description 6
- 238000005903 acid hydrolysis reaction Methods 0.000 claims 1
- 239000002904 solvent Substances 0.000 description 61
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 55
- -1 glycidoxy group Chemical group 0.000 description 49
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 36
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 33
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 32
- 150000001875 compounds Chemical class 0.000 description 32
- 125000000217 alkyl group Chemical group 0.000 description 31
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 24
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 23
- 150000003377 silicon compounds Chemical class 0.000 description 22
- 238000000034 method Methods 0.000 description 21
- 125000000524 functional group Chemical group 0.000 description 20
- 239000000178 monomer Substances 0.000 description 20
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- 238000005406 washing Methods 0.000 description 19
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 description 18
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- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 17
- 230000032683 aging Effects 0.000 description 17
- 239000002585 base Substances 0.000 description 17
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 17
- 125000003118 aryl group Chemical group 0.000 description 15
- 239000000499 gel Substances 0.000 description 14
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 13
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- 238000001879 gelation Methods 0.000 description 13
- 238000005259 measurement Methods 0.000 description 13
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- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 11
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- 125000004432 carbon atom Chemical group C* 0.000 description 11
- 239000003960 organic solvent Substances 0.000 description 11
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 10
- IMNFDUFMRHMDMM-UHFFFAOYSA-N N-Heptane Chemical compound CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 description 10
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- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 10
- 239000000377 silicon dioxide Substances 0.000 description 10
- 238000006467 substitution reaction Methods 0.000 description 10
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 9
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 9
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 9
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 8
- XTHFKEDIFFGKHM-UHFFFAOYSA-N Dimethoxyethane Chemical compound COCCOC XTHFKEDIFFGKHM-UHFFFAOYSA-N 0.000 description 8
- 238000004140 cleaning Methods 0.000 description 8
- 239000000126 substance Substances 0.000 description 8
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 7
- 125000003277 amino group Chemical group 0.000 description 7
- 230000015572 biosynthetic process Effects 0.000 description 7
- 238000006243 chemical reaction Methods 0.000 description 7
- 230000008569 process Effects 0.000 description 7
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 7
- 125000003396 thiol group Chemical group [H]S* 0.000 description 7
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 7
- AFABGHUZZDYHJO-UHFFFAOYSA-N 2-Methylpentane Chemical compound CCCC(C)C AFABGHUZZDYHJO-UHFFFAOYSA-N 0.000 description 6
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 6
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 6
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 6
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 6
- 125000002947 alkylene group Chemical group 0.000 description 6
- 125000004093 cyano group Chemical group *C#N 0.000 description 6
- XBDQKXXYIPTUBI-UHFFFAOYSA-N dimethylselenoniopropionate Natural products CCC(O)=O XBDQKXXYIPTUBI-UHFFFAOYSA-N 0.000 description 6
- 239000000203 mixture Substances 0.000 description 6
- 125000000449 nitro group Chemical group [O-][N+](*)=O 0.000 description 6
- 229910052710 silicon Inorganic materials 0.000 description 6
- 239000007787 solid Substances 0.000 description 6
- 125000001424 substituent group Chemical group 0.000 description 6
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 5
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 5
- 239000000908 ammonium hydroxide Substances 0.000 description 5
- 239000001569 carbon dioxide Substances 0.000 description 5
- 229910002092 carbon dioxide Inorganic materials 0.000 description 5
- YYLGKUPAFFKGRQ-UHFFFAOYSA-N dimethyldiethoxysilane Chemical compound CCO[Si](C)(C)OCC YYLGKUPAFFKGRQ-UHFFFAOYSA-N 0.000 description 5
- 235000019253 formic acid Nutrition 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 239000012046 mixed solvent Substances 0.000 description 5
- 229920000642 polymer Polymers 0.000 description 5
- 239000011164 primary particle Substances 0.000 description 5
- 125000005372 silanol group Chemical group 0.000 description 5
- GXDHCNNESPLIKD-UHFFFAOYSA-N 2-methylhexane Chemical compound CCCCC(C)C GXDHCNNESPLIKD-UHFFFAOYSA-N 0.000 description 4
- KWIUHFFTVRNATP-UHFFFAOYSA-N Betaine Natural products C[N+](C)(C)CC([O-])=O KWIUHFFTVRNATP-UHFFFAOYSA-N 0.000 description 4
- RGSFGYAAUTVSQA-UHFFFAOYSA-N Cyclopentane Chemical compound C1CCCC1 RGSFGYAAUTVSQA-UHFFFAOYSA-N 0.000 description 4
- OFOBLEOULBTSOW-UHFFFAOYSA-N Malonic acid Chemical compound OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 description 4
- KWIUHFFTVRNATP-UHFFFAOYSA-O N,N,N-trimethylglycinium Chemical compound C[N+](C)(C)CC(O)=O KWIUHFFTVRNATP-UHFFFAOYSA-O 0.000 description 4
- URLKBWYHVLBVBO-UHFFFAOYSA-N Para-Xylene Chemical group CC1=CC=C(C)C=C1 URLKBWYHVLBVBO-UHFFFAOYSA-N 0.000 description 4
- OFBQJSOFQDEBGM-UHFFFAOYSA-N Pentane Chemical compound CCCCC OFBQJSOFQDEBGM-UHFFFAOYSA-N 0.000 description 4
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 4
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 4
- DKGAVHZHDRPRBM-UHFFFAOYSA-N Tert-Butanol Chemical compound CC(C)(C)O DKGAVHZHDRPRBM-UHFFFAOYSA-N 0.000 description 4
- 230000002378 acidificating effect Effects 0.000 description 4
- 150000001338 aliphatic hydrocarbons Chemical class 0.000 description 4
- 229960003237 betaine Drugs 0.000 description 4
- 238000009835 boiling Methods 0.000 description 4
- 239000008119 colloidal silica Substances 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 150000002170 ethers Chemical class 0.000 description 4
- 125000001301 ethoxy group Chemical group [H]C([H])([H])C([H])([H])O* 0.000 description 4
- 238000005227 gel permeation chromatography Methods 0.000 description 4
- 125000002768 hydroxyalkyl group Chemical group 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- IVSZLXZYQVIEFR-UHFFFAOYSA-N m-xylene Chemical group CC1=CC=CC(C)=C1 IVSZLXZYQVIEFR-UHFFFAOYSA-N 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N monobenzene Natural products C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 4
- FDPIMTJIUBPUKL-UHFFFAOYSA-N pentan-3-one Chemical compound CCC(=O)CC FDPIMTJIUBPUKL-UHFFFAOYSA-N 0.000 description 4
- YWAKXRMUMFPDSH-UHFFFAOYSA-N pentene Chemical compound CCCC=C YWAKXRMUMFPDSH-UHFFFAOYSA-N 0.000 description 4
- 229920001451 polypropylene glycol Polymers 0.000 description 4
- 239000011148 porous material Substances 0.000 description 4
- VZGDMQKNWNREIO-UHFFFAOYSA-N tetrachloromethane Chemical compound ClC(Cl)(Cl)Cl VZGDMQKNWNREIO-UHFFFAOYSA-N 0.000 description 4
- LFQCEHFDDXELDD-UHFFFAOYSA-N tetramethyl orthosilicate Chemical compound CO[Si](OC)(OC)OC LFQCEHFDDXELDD-UHFFFAOYSA-N 0.000 description 4
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 description 3
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 description 3
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 description 3
- 239000002253 acid Substances 0.000 description 3
- 150000001412 amines Chemical class 0.000 description 3
- BTANRVKWQNVYAZ-UHFFFAOYSA-N butan-2-ol Chemical compound CCC(C)O BTANRVKWQNVYAZ-UHFFFAOYSA-N 0.000 description 3
- 239000004202 carbamide Substances 0.000 description 3
- 150000001732 carboxylic acid derivatives Chemical class 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
- UAOMVDZJSHZZME-UHFFFAOYSA-N diisopropylamine Chemical compound CC(C)NC(C)C UAOMVDZJSHZZME-UHFFFAOYSA-N 0.000 description 3
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- 125000003700 epoxy group Chemical group 0.000 description 3
- 238000011156 evaluation Methods 0.000 description 3
- 238000004108 freeze drying Methods 0.000 description 3
- RAXXELZNTBOGNW-UHFFFAOYSA-N imidazole Natural products C1=CNC=N1 RAXXELZNTBOGNW-UHFFFAOYSA-N 0.000 description 3
- 125000000956 methoxy group Chemical group [H]C([H])([H])O* 0.000 description 3
- BFXIKLCIZHOAAZ-UHFFFAOYSA-N methyltrimethoxysilane Chemical compound CO[Si](C)(OC)OC BFXIKLCIZHOAAZ-UHFFFAOYSA-N 0.000 description 3
- 239000013500 performance material Substances 0.000 description 3
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- IUVKMZGDUIUOCP-BTNSXGMBSA-N quinbolone Chemical compound O([C@H]1CC[C@H]2[C@H]3[C@@H]([C@]4(C=CC(=O)C=C4CC3)C)CC[C@@]21C)C1=CCCC1 IUVKMZGDUIUOCP-BTNSXGMBSA-N 0.000 description 3
- HNAGHMKIPMKKBB-UHFFFAOYSA-N 1-benzylpyrrolidine-3-carboxamide Chemical compound C1C(C(=O)N)CCN1CC1=CC=CC=C1 HNAGHMKIPMKKBB-UHFFFAOYSA-N 0.000 description 2
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- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical class [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
- LRXTYHSAJDENHV-UHFFFAOYSA-H zinc phosphate Chemical compound [Zn+2].[Zn+2].[Zn+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O LRXTYHSAJDENHV-UHFFFAOYSA-H 0.000 description 1
- 229910000165 zinc phosphate Inorganic materials 0.000 description 1
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- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/14—Colloidal silica, e.g. dispersions, gels, sols
- C01B33/157—After-treatment of gels
- C01B33/158—Purification; Drying; Dehydrating
- C01B33/1585—Dehydration into aerogels
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- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/16—Preparation of silica xerogels
- C01B33/163—Preparation of silica xerogels by hydrolysis of organosilicon compounds, e.g. ethyl orthosilicate
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- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/14—Colloidal silica, e.g. dispersions, gels, sols
- C01B33/145—Preparation of hydroorganosols, organosols or dispersions in an organic medium
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- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/14—Colloidal silica, e.g. dispersions, gels, sols
- C01B33/146—After-treatment of sols
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- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/14—Colloidal silica, e.g. dispersions, gels, sols
- C01B33/155—Preparation of hydroorganogels or organogels
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- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/16—Preparation of silica xerogels
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/32—Thermal properties
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- Silicon Polymers (AREA)
- Silicon Compounds (AREA)
Description
本実施形態に係るエアロゲルの製造方法は、シランオリゴマーを加水分解して、当該シランオリゴマーの加水分解生成物を含有するゾルを生成するゾル生成工程と、ゾルをゲル化して、湿潤ゲルを得る湿潤ゲル生成工程と、湿潤ゲルを乾燥してエアロゲルを得る乾燥工程と、を備える。この製造方法において、シランオリゴマー中のケイ素原子の総数に対する、3個の酸素原子と結合したケイ素原子の割合は、50%以上である。
ゾル生成工程は、シランオリゴマーを加水分解して、シランオリゴマーの加水分解生成物を含むゾルを生成する工程である。
湿潤ゲル生成工程は、ゾル生成工程で得られたゾルをゲル化して、湿潤ゲルを得る工程である。本工程は、ゾルをゲル化し、その後熟成して湿潤ゲルを得る工程であってもよい。本工程では、ゲル化を促進させるため塩基触媒を用いることができる。
洗浄工程は、湿潤ゲル生成工程で得られた湿潤ゲルを洗浄する工程である。洗浄工程では、湿潤ゲル中の洗浄液を乾燥条件(後述の乾燥工程)に適した溶媒に置換する溶媒置換を更に行ってもよい。
乾燥工程では、(必要に応じて洗浄工程を経た)湿潤ゲルを乾燥させることにより、エアロゲルを得ることができる。すなわち、上記ゾルから生成された湿潤ゲルを乾燥してなるエアロゲルを得ることができる。
本実施形態に係るエアロゲルは、シランオリゴマーを含有するゾルの縮合物である湿潤ゲルの乾燥物である。本実施形態に係るエアロゲルは、例えば、上述の製造方法によって得られたものであってよい。
本実施形態に係るエアロゲルは、下記一般式(1)で表される構造を有することができる。本実施形態に係るエアロゲルは、式(1)で表される構造を含む構造として、下記一般式(1a)で表される構造を有することができる。
本実施形態に係るエアロゲルは、支柱部及び橋かけ部を備えるラダー型構造を有し、かつ橋かけ部が下記一般式(2)で表される構造を有することができる。このようなラダー型構造をエアロゲル成分としてエアロゲルの骨格中に導入することにより、耐熱性と機械的強度を向上させることができる。なお、本実施形態において「ラダー型構造」とは、2本の支柱部(struts)と支柱部同士を連結する橋かけ部(bridges)とを有するもの(いわゆる「梯子」の形態を有するもの)である。本態様において、エアロゲルの骨格がラダー型構造からなっていてもよいが、エアロゲルが部分的にラダー型構造を有していてもよい。
本実施形態に係るエアロゲルは、さらに強靱化する観点並びにさらに優れた断熱性及び柔軟性を達成する観点から、エアロゲル成分に加え、さらにシリカ粒子を含有していてもよい。エアロゲル成分及びシリカ粒子を含有するエアロゲルを、エアロゲル複合体ということもできる。エアロゲル複合体は、エアロゲル成分とシリカ粒子とが複合化されていながらも、エアロゲルの特徴であるクラスター構造を有しており、三次元的に微細な多孔性の構造を有していると考えられる。
シランオリゴマーとして「XR31-B1410」(モメンティブ・パフォーマンス・マテリアルズ・ジャパン合同会社製、製品名)を100質量部、シランモノマーとしてテトラエトキシシラン「KBE-04」(信越化学工業株式会社製、製品名、以下「TEOS」と略記)を50質量部、2-プロパノールを300質量部、及び、水を100質量部混合し、これに酸触媒として酢酸を0.1質量部加え、25℃で4時間反応させてゾルを得た。得られたゾルに塩基触媒として5%濃度のアンモニア水を80質量部加え、60℃で1時間ゲル化した後、60℃で48時間熟成して湿潤ゲルを得た。その後、得られた湿潤ゲルを、常圧下にて、25℃で72時間乾燥し、その後150℃で2時間乾燥することで、エアロゲルを得た。
シランオリゴマーとして「SR-2402」(東レ・ダウコーニング株式会社製、製品名)を用いたこと以外は、実施例1と同様にしてエアロゲルを作製した。
シランオリゴマーとして「AY42-163」(東レ・ダウコーニング株式会社製、製品名)を用いたこと以外は、実施例1と同様にしてエアロゲルを作製した。
シランオリゴマーとして「KC-89S」(信越化学工業株式会社製、製品名)を100質量部、2-プロパノールを200質量部、及び、水を50質量部混合し、これに酸触媒として酢酸を0.15質量部加え、25℃で4時間反応させてゾルを得た。得られたゾルに塩基触媒として5%濃度のアンモニア水を60質量部加え、60℃で1時間ゲル化した後、60℃で48時間熟成して湿潤ゲルを得た。その後は、実施例1と同様にしてエアロゲルを作製した。
シランオリゴマーとして「KR-500」(信越化学工業株式会社製、製品名)を100質量部、シランモノマーとしてテトラエトキシシラン「KBE-04」(信越化学工業株式会社製、製品名、以下「TEOS」と略記)を100質量部、2-プロパノールを250質量部、及び、水を80質量部混合し、これに酸触媒として酢酸を0.15質量部加え、25℃で4時間反応させてゾルを得た。得られたゾルに塩基触媒として5%濃度のアンモニア水を90質量部加え、60℃で1時間ゲル化した後、60℃で48時間熟成して湿潤ゲルを得た。その後は、実施例1と同様にしてエアロゲルを作製した。
シランオリゴマーとして「KR-515」(信越化学工業株式会社製、製品名)を100質量部、シランモノマーとしてテトラエトキシシラン「KBE-04」(信越化学工業株式会社製、製品名、以下「TEOS」と略記)を20質量部、ジメチルジエトキシシラン「KBE-22」(信越化学工業株式会社製、製品名、以下「DMDES」と略記)を20質量部、2-プロパノールを300質量部、及び、水を80質量部混合し、これに酸触媒として酢酸を0.12質量部加え、25℃で4時間反応させてゾルを得た。得られたゾルに塩基触媒として5%濃度のアンモニア水を90質量部加え、60℃で1時間ゲル化した後、60℃で48時間熟成して湿潤ゲルを得た。その後は、実施例1と同様にしてエアロゲルを作製した。
シランオリゴマーとして「XR31-B1410」(モメンティブ・パフォーマンス・マテリアルズ・ジャパン合同会社製、製品名)を100質量部、ジメチルジエトキシシラン「KBE-22」(信越化学工業株式会社製、製品名、以下「DMDES」と略記)を70質量部、2-プロパノールを300質量部、及び、水を80質量部混合し、これに酸触媒として酢酸を0.1質量部加え、25℃で4時間反応させてゾルを得た。得られたゾルに塩基触媒として5%濃度のアンモニア水を80質量部加え、60℃で1時間ゲル化した後、60℃で48時間熟成して湿潤ゲルを得た。その後は、実施例1と同様にしてエアロゲルを作製した。
シランオリゴマーとして「XR31-B1410」(モメンティブ・パフォーマンス・マテリアルズ・ジャパン合同会社製、製品名)を100質量部、メチルトリメトキシシラン「KBM-13」(信越化学工業株式会社製、製品名、以下「MTMS」と略記)を200質量部、テトラエトキシシラン「KBE-04」(信越化学工業株式会社製、製品名、以下「TEOS」と略記)を50質量部、2-プロパノールを800質量部、及び、水を200質量部混合し、これに酸触媒として酢酸を0.5質量部加え、25℃で4時間反応させてゾルを得た。得られたゾルに塩基触媒として5%濃度のアンモニア水を200質量部加え、60℃で1時間ゲル化した後、60℃で48時間熟成して湿潤ゲルを得た。その後は、実施例1と同様にしてエアロゲルを作製した。
シランオリゴマーに代えて、シランモノマーであるメチルトリメトキシシラン「KBM-13」(信越化学工業株式会社製、製品名:以下「MTMS」と略記)を用いたこと以外は、実施例1と同様にしてエアロゲルを作製した。
シランオリゴマーに代えて、「メチルシリケート51」(T単位を有さず、Q単位のみで構成されたシランオリゴマー、コルコート株式会社製、製品名)に変更したこと以外は、実施例1と同様にしてエアロゲルを作製した。
各実施例及び比較例で得られたエアロゲルについて、以下の条件に従って外観観察、体積収縮率測定、密度測定及び熱伝導率測定を行い、評価した。評価結果を表1に示す。
得られたエアロゲルにおいて、湿潤ゲルと同様の形状を保っているものを「A」とし、クラック等で形状が保たれていないものを「C」とした。
得られたエアロゲルにおいて、下記の式により体積収縮率を算出した。体積収縮率が20%未満のものを「A」、20%以上のものを「C」とした。
体積収縮率[%]=[(乾燥ゲルの体積)/(湿潤ゲルの体積)]×100
水中置換法に従い、電子比重計(アルファミラージュ株式会社製、製品名SD-200L)を用いてエアロゲルの密度を測定した。
刃角約20~25度の刃を用いて、エアロゲルを150×150×100mm3のサイズに加工し、測定サンプルとした。次に、面の平行を確保するために、必要に応じて#1500以上の紙やすりで整形した。得られた測定サンプルを、熱伝導率測定前に、定温乾燥機「DVS402」(ヤマト科学株式会社製、製品名)を用いて、大気圧下、100℃で30分間乾燥した。次いで測定サンプルをデシケータ中に移し、25℃まで冷却した。
RS=N((TU-TL)/Q)-RO
式中、TUは測定サンプル上面温度を示し、TLは測定サンプル下面温度を示し、ROは上下界面の接触熱抵抗を示し、Qは熱流束計出力を示す。なお、Nは比例係数であり、較正試料を用いて予め求めておいた。
λ=d/RS
式中、dは測定サンプルの厚さを示す。
Claims (4)
- シランオリゴマーを酸触媒で加水分解して、前記シランオリゴマーの加水分解生成物を含有するゾルを生成するゾル生成工程と、
前記ゾルを塩基触媒でゲル化して、湿潤ゲルを得る湿潤ゲル生成工程と、
前記湿潤ゲルを乾燥してエアロゲルを得る乾燥工程と、
を備え、
前記シランオリゴマー中のケイ素原子の総数に対する、3個の酸素原子と結合したケイ素原子の割合が50%以上であり、
前記シランオリゴマーの重量平均分子量が200以上10000以下である、エアロゲルの製造方法。 - 前記シランオリゴマーがアルコキシ基を有し、
前記アルコキシ基の含有量が、前記シランオリゴマーの全量基準で、2質量%以上60質量%以下である、請求項1に記載の製造方法。 - シランオリゴマーの酸加水分解生成物を含有するゾルの縮合物である湿潤ゲルの乾燥物であって、
前記シランオリゴマー中のケイ素原子の総数に対する、3個の酸素原子と結合したケイ素原子の割合が50%以上であり、
前記シランオリゴマーの重量平均分子量が200以上10000以下である、エアロゲル。 - 前記シランオリゴマーがアルコキシ基を有し、
前記アルコキシ基の含有量が、前記シランオリゴマーの全量基準で2質量%以上60質量%以下である、請求項3に記載のエアロゲル。
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