JP6611916B2 - シリカエアロゲルを含むブランケット及びこの製造方法 - Google Patents
シリカエアロゲルを含むブランケット及びこの製造方法 Download PDFInfo
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- JP6611916B2 JP6611916B2 JP2018511383A JP2018511383A JP6611916B2 JP 6611916 B2 JP6611916 B2 JP 6611916B2 JP 2018511383 A JP2018511383 A JP 2018511383A JP 2018511383 A JP2018511383 A JP 2018511383A JP 6611916 B2 JP6611916 B2 JP 6611916B2
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- Prior art keywords
- blanket
- silica airgel
- silica
- opacifying agent
- inorganic particles
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- 239000011572 manganese Substances 0.000 description 1
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- BFXIKLCIZHOAAZ-UHFFFAOYSA-N methyltrimethoxysilane Chemical compound CO[Si](C)(OC)OC BFXIKLCIZHOAAZ-UHFFFAOYSA-N 0.000 description 1
- 229910021382 natural graphite Inorganic materials 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 150000002843 nonmetals Chemical class 0.000 description 1
- HMMGMWAXVFQUOA-UHFFFAOYSA-N octamethylcyclotetrasiloxane Chemical compound C[Si]1(C)O[Si](C)(C)O[Si](C)(C)O[Si](C)(C)O1 HMMGMWAXVFQUOA-UHFFFAOYSA-N 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- HJGMWXTVGKLUAQ-UHFFFAOYSA-N oxygen(2-);scandium(3+) Chemical compound [O-2].[O-2].[O-2].[Sc+3].[Sc+3] HJGMWXTVGKLUAQ-UHFFFAOYSA-N 0.000 description 1
- 238000007415 particle size distribution analysis Methods 0.000 description 1
- 239000005011 phenolic resin Substances 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 description 1
- 229920002647 polyamide Polymers 0.000 description 1
- 229920002480 polybenzimidazole Polymers 0.000 description 1
- 229920005594 polymer fiber Polymers 0.000 description 1
- 229920000098 polyolefin Polymers 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 1
- 239000004810 polytetrafluoroethylene Substances 0.000 description 1
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000013557 residual solvent Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 229910000077 silane Inorganic materials 0.000 description 1
- SCPYDCQAZCOKTP-UHFFFAOYSA-N silanol Chemical compound [SiH3]O SCPYDCQAZCOKTP-UHFFFAOYSA-N 0.000 description 1
- 125000005372 silanol group Chemical group 0.000 description 1
- 150000004760 silicates Chemical class 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- 239000000600 sorbitol Substances 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 229910001256 stainless steel alloy Inorganic materials 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 150000005846 sugar alcohols Polymers 0.000 description 1
- FGWRMMTYIZKYMA-UHFFFAOYSA-N tert-butyl-hydroxy-dimethylsilane Chemical compound CC(C)(C)[Si](C)(C)O FGWRMMTYIZKYMA-UHFFFAOYSA-N 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- 239000006234 thermal black Substances 0.000 description 1
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 1
- 229910001887 tin oxide Inorganic materials 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- 235000019976 tricalcium silicate Nutrition 0.000 description 1
- 229910021534 tricalcium silicate Inorganic materials 0.000 description 1
- WVMSIBFANXCZKT-UHFFFAOYSA-N triethyl(hydroxy)silane Chemical compound CC[Si](O)(CC)CC WVMSIBFANXCZKT-UHFFFAOYSA-N 0.000 description 1
- ZNOCGWVLWPVKAO-UHFFFAOYSA-N trimethoxy(phenyl)silane Chemical compound CO[Si](OC)(OC)C1=CC=CC=C1 ZNOCGWVLWPVKAO-UHFFFAOYSA-N 0.000 description 1
- AAPLIUHOKVUFCC-UHFFFAOYSA-N trimethylsilanol Chemical compound C[Si](C)(C)O AAPLIUHOKVUFCC-UHFFFAOYSA-N 0.000 description 1
- NLSXASIDNWDYMI-UHFFFAOYSA-N triphenylsilanol Chemical compound C=1C=CC=CC=1[Si](C=1C=CC=CC=1)(O)C1=CC=CC=C1 NLSXASIDNWDYMI-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
- 238000009834 vaporization Methods 0.000 description 1
- 230000008016 vaporization Effects 0.000 description 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
- 239000011800 void material Substances 0.000 description 1
Classifications
-
- 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
- C04B30/00—Compositions for artificial stone, not containing binders
- C04B30/02—Compositions for artificial stone, not containing binders containing fibrous materials
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- 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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- C01B33/00—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
- C01B33/159—Coating or hydrophobisation
-
- 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
- C01G23/047—Titanium dioxide
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K7/00—Constructional details common to different types of electric apparatus
- H05K7/20—Modifications to facilitate cooling, ventilating, or heating
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/02—Solvent extraction of solids
- B01D11/0203—Solvent extraction of solids with a supercritical fluid
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/88—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by thermal analysis data, e.g. TGA, DTA, DSC
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- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
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- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01P2006/12—Surface area
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- C01P2006/40—Electric properties
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- C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
- C04B2111/20—Resistance against chemical, physical or biological attack
- C04B2111/28—Fire resistance, i.e. materials resistant to accidental fires or high temperatures
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- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/02—Polysilicates
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- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/14—Polysiloxanes containing silicon bound to oxygen-containing groups
- C08G77/18—Polysiloxanes containing silicon bound to oxygen-containing groups to alkoxy or aryloxy groups
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- H—ELECTRICITY
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- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L23/00—Details of semiconductor or other solid state devices
- H01L23/34—Arrangements for cooling, heating, ventilating or temperature compensation ; Temperature sensing arrangements
- H01L23/36—Selection of materials, or shaping, to facilitate cooling or heating, e.g. heatsinks
- H01L23/373—Cooling facilitated by selection of materials for the device or materials for thermal expansion adaptation, e.g. carbon
- H01L23/3737—Organic materials with or without a thermoconductive filler
Description
本出願は、2015年9月10日付韓国特許出願第2015-0128547号及び2016年3月28日付韓国特許出願第2016-0036566号に基づく優先権の利益を主張し、当該韓国特許出願の文献に開示された全ての内容は本明細書の一部として含まれる。
ルチル型結晶性を有するTiO2 5gを2M 水酸化カリウム(KOH)溶液に入れて3時間の間撹拌してTiO2に対するエッチング反応を行った。 結果のエッチング液に水240mlを添加して精製して水中にエッチングされたTiO2が分散された不透明化剤を含む分散液を製造した。
前記実施例1でポリエチレンテレフタレート(PET)ファイバーの代りに、ヘキサメチルジシラザン(HMDS)で疎水化表面処理したPETファイバーを用いることを除いては、前記実施例1と同じ方法で行ってブランケットを製造した。
シリカアルコキシド前駆体20gとエタノール40gを混合して製造した前駆体溶液に、不透明化剤としてルチル型結晶性を有するTiO2 5gを蒸留水240mlに分散させて製造した分散液5mlを添加して不透明化剤を含む−シリカエアロゲル形成用組成物を製造した。前記不透明化剤を含む−シリカエアロゲル形成用組成物に、アンモニア触媒0.5mlをエタノール12mlで希釈した溶液を前記組成物のpHが8〜9となるように添加し、PETファイバーにキャスティングしてゲル化を誘導した。ゲル化を完了した後、結果として収得された不透明化剤−シリカゲル−基材複合剤を2.0重量%のアンモニア水溶液を用いて50℃から70分間エージングした。エージング完了後、結果の不透明化剤−シリカゲル−基材複合剤に対して、ヘキサメチルジシラザン(HMDS)4mlとエタノール 76mlを混合して製造した表面改質剤含有溶液80mlを用いて12時間の間疎水化表面改質を行った。疎水化表面改質反応の完了後、結果として収得された湿潤ゲルを常圧(1atm)乾燥し、シリカエアロゲル及び不透明化剤が含まれたブランケットを製造した。
前記実施例1及び比較例1で製造した不透明化剤を透過電子顕微鏡を用いて観察した。その結果を図1及び2にそれぞれ示した。
不透明化剤のエッチング時に塩基物質の使用量による平均粒子直径及び平均ゼータ電位の変化を観察した。
前記実施例1及び比較例1で製造した不透明化剤の分散性を評価した。
前記実施例1及び比較例1で製造したシリカエアロゲルを含むブランケットに対して平均重量損失、熱伝導度(T/C)及び真密度をそれぞれ測定した。その結果を下記表 2に示した。
前記実施例1及び比較例1で製造したシリカエアロゲルを含むブランケット内のシリカエアロゲルの比表面積、シリカエアロゲル内の総気孔体積(total pore volume)及び平均気孔直径(avg. pore diameter)を3Flex(Micromeritics社製)を用いてそれぞれ測定した。その結果を下記表 3に示した。
前記実施例1及び比較例1で製造したシリカエアロゲルを含むブランケットに対して、高温処理による疎水性変化を観察した。
Claims (16)
- ブランケット用基材;及び
前記ブランケット用基材の表面及び内部のうち少なくとも一つに位置する、シリカエアロゲル及び不透明化剤を含み、
前記不透明化剤は、1次粒子状の無機粒子が凝集された2次粒子状であり、1μm3単位体積当たり1個から5個の無機粒子を含むシリカエアロゲルを含むブランケット。 - 前記不透明化剤は、平均粒子直径が300nmから1600nmである請求項1に記載のシリカエアロゲルを含むブランケット。
- 前記無機粒子は、粒子表面にヒドロキシル基、アルコキシ基、カルボキシル基及びエステル基からなる群より選択されるいずれか一つまたは二つ以上の縮合反応性官能基を含む請求項1または2に記載のシリカエアロゲルを含むブランケット。
- 前記無機粒子は、表面上に凹凸を有する請求項1〜3のいずれか一項に記載のシリカエアロゲルを含むブランケット。
- 前記無機粒子は、金属酸化物、金属炭化物、金属窒化物、金属水酸化物、金属塩、炭素系物質、セラミック粒子及びこれらの混合物からなる群より選択されるいずれか一つまたは二つ以上を含む請求項1〜4のいずれか一項に記載のシリカエアロゲルを含むブランケット。
- 前記無機粒子は、ルチル型TiO2及びアナターゼ型TiO2からなる群より選択される少なくともいずれか一つのチタニウム酸化物を含む請求項1〜5のいずれか一項に記載のシリカエアロゲルを含むブランケット。
- 前記シリカエアロゲルは、1次粒子等が結合された3次元網目構造を有する請求項1〜6のいずれか一項に記載のシリカエアロゲルを含むブランケット。
- 前記シリカエアロゲルは、比表面積が700m2/g以上である請求項1〜7のいずれか一項に記載のシリカエアロゲルを含むブランケット。
- 前記シリカエアロゲルは、シリカエアロゲルの総重量に対して8重量%以上の炭素含量を有する疎水性シリカエアロゲルである請求項1〜8のいずれか一項に記載のシリカエアロゲルを含むブランケット。
- 前記ブランケット用基材は、基材の少なくとも一面に疎水性表面処理層をさらに含む請求項1〜9のいずれか一項に記載のシリカエアロゲルを含むブランケット。
- 前記不透明化剤は、シリカエアロゲルに化学結合して不透明化剤−シリカエアロゲル複合体を形成する請求項1〜10のいずれか一項に記載のシリカエアロゲルを含むブランケット。
- 無機粒子を塩基性水溶液中に分散させてエッチングした後、水を添加して不透明化剤を含む分散液を準備する段階;
前記不透明化剤を含む分散液をシリカ前駆体と混合し、不透明化剤を含むシリカエアロゲル形成用組成物を準備する段階;
前記不透明化剤を含むシリカエアロゲル形成用組成物に、塩基触媒及び極性有機溶媒を添加した後、ブランケット用基材を添加してゲル化させ、不透明化剤−シリカゲル−基材複合体を準備する段階;及び
前記不透明化剤−シリカゲル−基材複合体を疎水化表面改質処理した後、乾燥する段階
を含むシリカエアロゲルを含むブランケットの製造方法。 - 前記塩基性水溶液は、12以上の酸解離定数値を有する強塩基及び水を含む請求項12に記載のシリカエアロゲルを含むブランケットの製造方法。
- 前記エッチングは、12以上の酸解離定数値を有する強塩基を0.1Mから10Mの濃度で含む塩基性水溶液中に無機粒子を分散させた後、最終製造される不透明化剤を含む分散液中での不透明化剤が−10mVから−60mVの平均ゼータ電位を示すようにする時間の間行われる請求項12または13に記載のシリカエアロゲルを含むブランケットの製造方法。
- 前記疎水化表面改質処理は、分子内2個以上のアルキル基を含むシラザン系表面改質剤を用いて行われる請求項12〜14のいずれか一項に記載のシリカエアロゲルを含むブランケットの製造方法。
- 請求項1から請求項11のいずれか一項に記載のシリカエアロゲルを含むブランケットを含む断熱材。
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