JPWO2011118252A1 - シリカ膜の製造方法 - Google Patents
シリカ膜の製造方法 Download PDFInfo
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- JPWO2011118252A1 JPWO2011118252A1 JP2011541427A JP2011541427A JPWO2011118252A1 JP WO2011118252 A1 JPWO2011118252 A1 JP WO2011118252A1 JP 2011541427 A JP2011541427 A JP 2011541427A JP 2011541427 A JP2011541427 A JP 2011541427A JP WO2011118252 A1 JPWO2011118252 A1 JP WO2011118252A1
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 109
- 239000000377 silicon dioxide Substances 0.000 title claims abstract description 54
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 19
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims abstract description 50
- 239000000758 substrate Substances 0.000 claims abstract description 41
- 238000007664 blowing Methods 0.000 claims abstract description 11
- 238000010304 firing Methods 0.000 claims description 4
- 239000012528 membrane Substances 0.000 abstract description 50
- 230000004907 flux Effects 0.000 abstract description 9
- 239000010408 film Substances 0.000 description 75
- 238000000926 separation method Methods 0.000 description 28
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 22
- 239000000919 ceramic Substances 0.000 description 20
- 238000001035 drying Methods 0.000 description 20
- 230000015572 biosynthetic process Effects 0.000 description 18
- 210000004027 cell Anatomy 0.000 description 18
- 238000005755 formation reaction Methods 0.000 description 18
- 239000000243 solution Substances 0.000 description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 14
- 239000007788 liquid Substances 0.000 description 13
- 239000011148 porous material Substances 0.000 description 13
- 238000000034 method Methods 0.000 description 9
- 230000007547 defect Effects 0.000 description 8
- 239000011248 coating agent Substances 0.000 description 7
- 238000000576 coating method Methods 0.000 description 7
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 6
- 239000000463 material Substances 0.000 description 6
- 230000000873 masking effect Effects 0.000 description 5
- 230000002093 peripheral effect Effects 0.000 description 5
- 239000012466 permeate Substances 0.000 description 5
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 4
- 239000002904 solvent Substances 0.000 description 4
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 239000011552 falling film Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 238000005192 partition Methods 0.000 description 3
- 239000002344 surface layer Substances 0.000 description 3
- 238000009423 ventilation Methods 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 2
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 2
- 229910010293 ceramic material Inorganic materials 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000009833 condensation Methods 0.000 description 2
- 230000005494 condensation Effects 0.000 description 2
- 229910052878 cordierite Inorganic materials 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- JSKIRARMQDRGJZ-UHFFFAOYSA-N dimagnesium dioxido-bis[(1-oxido-3-oxo-2,4,6,8,9-pentaoxa-1,3-disila-5,7-dialuminabicyclo[3.3.1]nonan-7-yl)oxy]silane Chemical compound [Mg++].[Mg++].[O-][Si]([O-])(O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2)O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2 JSKIRARMQDRGJZ-UHFFFAOYSA-N 0.000 description 2
- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 description 2
- 239000010410 layer Substances 0.000 description 2
- 238000001471 micro-filtration Methods 0.000 description 2
- 229910052863 mullite Inorganic materials 0.000 description 2
- 229910017604 nitric acid Inorganic materials 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 2
- 229910010271 silicon carbide Inorganic materials 0.000 description 2
- 239000011550 stock solution Substances 0.000 description 2
- 239000010409 thin film Substances 0.000 description 2
- 235000006508 Nelumbo nucifera Nutrition 0.000 description 1
- 240000002853 Nelumbo nucifera Species 0.000 description 1
- 239000003929 acidic solution Substances 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 238000007605 air drying Methods 0.000 description 1
- 239000012670 alkaline solution Substances 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 238000000861 blow drying Methods 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 238000007791 dehumidification Methods 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- 238000001612 separation test Methods 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000000108 ultra-filtration Methods 0.000 description 1
- 238000009834 vaporization Methods 0.000 description 1
- 230000008016 vaporization Effects 0.000 description 1
Images
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/02—Inorganic material
- B01D71/024—Oxides
- B01D71/027—Silicium oxide
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0039—Inorganic membrane manufacture
- B01D67/0046—Inorganic membrane manufacture by slurry techniques, e.g. die or slip-casting
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0081—After-treatment of organic or inorganic membranes
- B01D67/0095—Drying
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/12—Composite membranes; Ultra-thin membranes
- B01D69/1213—Laminated layers
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2323/00—Details relating to membrane preparation
- B01D2323/08—Specific temperatures applied
- B01D2323/081—Heating
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
- Compositions Of Oxide Ceramics (AREA)
Abstract
Description
(1)多孔質基材
平均細孔径が10nmのチタニアのUF膜が形成されているモノリス形状(外径180mm,セル内径3mm×2000セル,長さ1000mm)の基材(多孔質基材11)を用いた。尚、基材両端部はガラスにてシールした。
テトラエトシキシランを硝酸の存在下で加水分解し、シリカゾル液を得た。上記シリカゾル液をエタノールで希釈し、シリカ換算で0.7質量%となるように調整しコーティング液(成膜用シリカゾル液)40とした。
多孔質基材11の外周面をマスキングテープ41でマスクした。多孔質基材11を流下製膜装置に固定した。流下製膜装置のタンクに成膜用シリカゾル液40を溜め、基材上部から成膜用シリカゾル液40を流し込みセル23内を通過させた。その後基材上部から風速5m/sの風を送り、余剰なシリカゾルを除去した。なお、この成膜工程により、内側壁の全体に成膜されることを確認した。
成膜用シリカゾル液40を流し込んでシリカゾルを付着させた多孔質基材11のセル23内を、30秒以内に除湿送風機30を用いて室温の風を通過させて30分間乾燥させた。なお、風速は、5〜20m/s、風露点は、−70〜0℃とした。また、比較例1〜2は、風露点が0℃より高い風を用いて乾燥させた。
多孔質基材11の外周面のマスキングテープを取り外し、電気炉で25℃/hrにて昇温し、500℃で1時間保持した後、25℃/hrで降温した。尚、上記(3)〜(5)の操作を2回繰り返して実施例の試料を得た。
水−エタノールの分離試験を行った。具体的には、12L/minの送液速度でシリカ膜1が形成されたモノリス(多孔質基材11)のセル23内を、温度70℃、エタノール濃度90質量%、水10質量%の水溶液を流通させた。このとき、基材側面から約2〜5Paの真空度で減圧し、基材側面からの透過液を液体窒素トラップで捕集した。トラップで捕集した透過液と透過前の原液のエタノール濃度から分離係数を算出した。また、分離係数及び透過流束を表1に示す。
Claims (2)
- 多孔質基材上にシリカゾルを付着させ、
露点が−70〜0℃の風を送風することにより前記シリカゾルを乾燥させ、
その後焼成することによりシリカ膜を製造するシリカ膜の製造方法。 - 前記風を風速5〜20m/sで送風することにより前記シリカゾルを乾燥させる請求項1に記載のシリカ膜の製造方法。
Priority Applications (1)
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JP2011541427A JP5897334B2 (ja) | 2010-03-24 | 2011-01-28 | シリカ膜の製造方法 |
Applications Claiming Priority (4)
Application Number | Priority Date | Filing Date | Title |
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JP2010067812 | 2010-03-24 | ||
JP2010067812 | 2010-03-24 | ||
PCT/JP2011/051718 WO2011118252A1 (ja) | 2010-03-24 | 2011-01-28 | シリカ膜の製造方法 |
JP2011541427A JP5897334B2 (ja) | 2010-03-24 | 2011-01-28 | シリカ膜の製造方法 |
Publications (2)
Publication Number | Publication Date |
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JPWO2011118252A1 true JPWO2011118252A1 (ja) | 2013-07-04 |
JP5897334B2 JP5897334B2 (ja) | 2016-03-30 |
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JP2011541427A Active JP5897334B2 (ja) | 2010-03-24 | 2011-01-28 | シリカ膜の製造方法 |
Country Status (4)
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US (1) | US9403130B2 (ja) |
EP (1) | EP2556882B1 (ja) |
JP (1) | JP5897334B2 (ja) |
WO (1) | WO2011118252A1 (ja) |
Families Citing this family (2)
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JP5829902B2 (ja) * | 2011-12-21 | 2015-12-09 | 日本碍子株式会社 | フィルタおよびその製造方法 |
WO2013145857A1 (ja) * | 2012-03-29 | 2013-10-03 | 日本碍子株式会社 | 分離膜の製造方法 |
Family Cites Families (13)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4990252A (en) * | 1987-02-04 | 1991-02-05 | Hydanautics | Stable membranes from sulfonated polyarylethers |
US5772735A (en) * | 1995-11-02 | 1998-06-30 | University Of New Mexico | Supported inorganic membranes |
US6536604B1 (en) * | 1999-06-25 | 2003-03-25 | C. Jeffrey Brinker | Inorganic dual-layer microporous supported membranes |
KR20020076246A (ko) * | 1999-12-23 | 2002-10-09 | 액센투스 피엘씨 | 미세다공성 막 |
JP2004168615A (ja) * | 2002-11-21 | 2004-06-17 | National Institute Of Advanced Industrial & Technology | 多孔質シリカ膜及びその製造方法 |
RU2422357C2 (ru) * | 2005-09-23 | 2011-06-27 | Мекс, Инк. | Катализаторы на основе оксида рутения для конверсии диоксида серы в триоксид серы |
JP5269583B2 (ja) * | 2006-02-16 | 2013-08-21 | 日本碍子株式会社 | セラミック多孔質膜の製造方法 |
US20080096751A1 (en) * | 2006-10-18 | 2008-04-24 | Ngk Insulators, Ltd. | Method of manufacturing ceramic porous membrane and method of manufacturing ceramic filter |
JP5048371B2 (ja) | 2007-03-29 | 2012-10-17 | 日本碍子株式会社 | セラミック多孔質膜の製造方法及びセラミックフィルタの製造方法 |
JP2009241054A (ja) * | 2008-03-12 | 2009-10-22 | Ngk Insulators Ltd | セラミックフィルタの製造方法 |
JP4960286B2 (ja) * | 2008-03-21 | 2012-06-27 | 日本碍子株式会社 | ナノ濾過膜の製造方法 |
JP2009263598A (ja) * | 2008-04-30 | 2009-11-12 | Fujifilm Corp | 有機−無機ハイブリッド自立膜、およびその製造方法 |
WO2010125898A1 (ja) * | 2009-05-01 | 2010-11-04 | 日本碍子株式会社 | 塩酸濃縮用分離膜、塩酸濃縮方法及び塩酸濃縮装置 |
-
2011
- 2011-01-28 EP EP11758358.3A patent/EP2556882B1/en active Active
- 2011-01-28 JP JP2011541427A patent/JP5897334B2/ja active Active
- 2011-01-28 WO PCT/JP2011/051718 patent/WO2011118252A1/ja active Application Filing
- 2011-09-23 US US13/242,552 patent/US9403130B2/en active Active
Also Published As
Publication number | Publication date |
---|---|
EP2556882A4 (en) | 2017-04-05 |
US20120009346A1 (en) | 2012-01-12 |
JP5897334B2 (ja) | 2016-03-30 |
US9403130B2 (en) | 2016-08-02 |
EP2556882B1 (en) | 2022-11-09 |
WO2011118252A1 (ja) | 2011-09-29 |
EP2556882A1 (en) | 2013-02-13 |
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