JP6767876B2 - 分離膜構造体及びその製造方法 - Google Patents
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- 238000000926 separation method Methods 0.000 title claims description 82
- 238000004519 manufacturing process Methods 0.000 title claims description 11
- 239000012528 membrane Substances 0.000 claims description 91
- 239000011521 glass Substances 0.000 claims description 63
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 claims description 23
- 229910021536 Zeolite Inorganic materials 0.000 claims description 19
- 239000010457 zeolite Substances 0.000 claims description 19
- 238000001035 drying Methods 0.000 claims description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- 239000002904 solvent Substances 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 239000002002 slurry Substances 0.000 description 53
- 238000010899 nucleation Methods 0.000 description 33
- 239000000463 material Substances 0.000 description 27
- 238000000034 method Methods 0.000 description 17
- 239000011148 porous material Substances 0.000 description 12
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 11
- 239000007788 liquid Substances 0.000 description 10
- 239000007789 gas Substances 0.000 description 9
- 239000000243 solution Substances 0.000 description 9
- 230000015572 biosynthetic process Effects 0.000 description 7
- 239000011230 binding agent Substances 0.000 description 6
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 description 5
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 5
- 239000000377 silicon dioxide Substances 0.000 description 5
- 238000003786 synthesis reaction Methods 0.000 description 5
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 4
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 description 4
- 229910004298 SiO 2 Inorganic materials 0.000 description 4
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 4
- DKNWSYNQZKUICI-UHFFFAOYSA-N amantadine Chemical compound C1C(C2)CC3CC2CC1(N)C3 DKNWSYNQZKUICI-UHFFFAOYSA-N 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 239000012530 fluid Substances 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 3
- 229910052753 mercury Inorganic materials 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 238000009423 ventilation Methods 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 2
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 229910002092 carbon dioxide Inorganic materials 0.000 description 2
- 239000001569 carbon dioxide Substances 0.000 description 2
- 229910010293 ceramic material Inorganic materials 0.000 description 2
- 229910052878 cordierite Inorganic materials 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000010586 diagram Methods 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
- 238000001125 extrusion Methods 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 238000010304 firing Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 238000001027 hydrothermal synthesis Methods 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 238000000465 moulding Methods 0.000 description 2
- 229910052863 mullite Inorganic materials 0.000 description 2
- 239000003002 pH adjusting agent Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000007789 sealing Methods 0.000 description 2
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000004094 surface-active agent Substances 0.000 description 2
- 238000009834 vaporization Methods 0.000 description 2
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 1
- WOLHOYHSEKDWQH-UHFFFAOYSA-N amantadine hydrochloride Chemical compound [Cl-].C1C(C2)CC3CC2CC1([NH3+])C3 WOLHOYHSEKDWQH-UHFFFAOYSA-N 0.000 description 1
- 229910002091 carbon monoxide Inorganic materials 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 239000004927 clay Substances 0.000 description 1
- 239000002734 clay mineral Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- 230000008595 infiltration Effects 0.000 description 1
- 238000001764 infiltration Methods 0.000 description 1
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 239000005011 phenolic resin Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 230000008016 vaporization Effects 0.000 description 1
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- 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
- B01D71/028—Molecular sieves
- B01D71/0281—Zeolites
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/22—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by diffusion
- B01D53/228—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by diffusion characterised by specific membranes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D63/00—Apparatus in general for separation processes using semi-permeable membranes
- B01D63/06—Tubular membrane modules
- B01D63/066—Tubular membrane modules with a porous block having membrane coated passages
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D65/00—Accessories or auxiliary operations, in general, for separation processes or apparatus using semi-permeable membranes
- B01D65/003—Membrane bonding or sealing
-
- 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
- B01D67/0039—Inorganic membrane manufacture
- B01D67/0051—Inorganic membrane manufacture by controlled crystallisation, e,.g. hydrothermal growth
-
- 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
- B01D69/04—Tubular membranes
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B39/00—Compounds having molecular sieve and base-exchange properties, e.g. crystalline zeolites; Their preparation; After-treatment, e.g. ion-exchange or dealumination
- C01B39/02—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof; Direct preparation thereof; Preparation thereof starting from a reaction mixture containing a crystalline zeolite of another type, or from preformed reactants; After-treatment thereof
- C01B39/46—Other types characterised by their X-ray diffraction pattern and their defined composition
- C01B39/48—Other types characterised by their X-ray diffraction pattern and their defined composition using at least one organic template directing agent
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/22—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by diffusion
- B01D2053/221—Devices
- B01D2053/223—Devices with hollow tubes
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01D2256/00—Main component in the product gas stream after treatment
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Description
図1は、分離膜構造体100の斜視図である。図2は、図1のA−A断面図である。
まず、多孔質材料を含む坏土を用いて、複数の第2貫通孔TH2が形成された基材111の成形体を形成する。基材111の成形体を形成する方法としては、真空押出成形機を用いた押出成形法のほかプレス成型法や鋳込み成型法を用いることができる。
以上、本発明の一実施形態について説明したが、本発明は上記実施形態に限定されるものではなく、発明の要旨を逸脱しない範囲で種々の変更が可能である。
以下のようにして、サンプルNo.1〜12に係る分離膜構造体を作製した。
まず、各サンプルのDDR型ゼオライト膜に二酸化炭素及びメタンの25℃の混合ガス(各ガスの体積比=50:50)を0.3MPaでセル内に導入し、ゼオライト膜を隔てた供給側と透過側のガス濃度を測定した。そして、次の式(1)に基づいて分離性能αを算出した。
(数1)
α=(透過側のCO2濃度/透過側のCH4濃度)/(供給側のCO2濃度/供給側のCH4濃度)・・・(1)
分離性能αの算出結果は表1に示す通りである。なお、表1に示される分離性能αは、所定値を基準として規格化された値である。
110 多孔質支持体
120 第1ガラスシール
121 第1シール本体部
122 第1延在部
130 第2ガラスシール
131 第2シール本体部
132 第2延在部
140 分離膜
141 第1接続部
142 第2接続部
TH1 第1貫通孔
Claims (9)
- 第1端面と第2端面に連なる貫通孔を有する多孔質支持体と、
前記第1端面を覆う第1ガラスシールと、
前記貫通孔の内表面上に形成される分離膜と、
を備え、
前記第1ガラスシールは、前記第1端面上に配置される第1シール本体部と、前記第1シール本体部に連なり、前記貫通孔の前記内表面上に配置される第1延在部とを有し、
前記分離膜は、前記第1ガラスシールの前記第1延在部に接続される第1接続部を有し、
前記第1接続部の少なくとも一部は、前記第1延在部上に配置され、
前記第1接続部の第1厚みは、10μm以下であり、かつ、前記分離膜の長手方向中央における中央厚みの1.4倍以下である、
分離膜構造体。 - 前記第2端面を覆う第2ガラスシールを備え、
前記第2ガラスシールは、前記第2端面上に配置される第2シール本体部と、前記第2シール本体部に連なり、前記貫通孔の前記内表面上に配置される第2延在部とを有し、
前記分離膜は、前記第2ガラスシールの前記第2延在部に接続される第2接続部を有し、
前記第2接続部の少なくとも一部は、前記第2延在部上に配置され、
前記第2接続部の第2厚みは、10μm以下であり、かつ、前記中央厚みの3.2倍以下である、
請求項1に記載の分離膜構造体。 - 前記第2厚みは、前記中央厚みの2.1倍以下である、
請求項2に記載の分離膜構造体。 - 前記分離膜は、ゼオライト膜である、
請求項1乃至3のいずれかに記載の分離膜構造体。 - 多孔質支持体の第1端面を覆う第1ガラスシールと、前記多孔質支持体の第2端面を覆う第2ガラスシールとを形成する工程と、
前記第1端面を前記第2端面よりも低くして、前記第1端面と前記第2端面に連なる貫通孔の内表面に、分離膜を形成するための溶液を付着する工程と、
前記第2端面を前記第1端面よりも低くして、前記第1端面側から前記第2端面側に向かって前記貫通孔内に気体を流すことによって前記溶液を乾燥させる工程と、
を備える分離膜構造体の製造方法。 - 前記分離膜は、ゼオライト膜であり、
前記溶液は、ゼオライト粒子と溶媒を含有している、
請求項5に記載の分離膜構造体の製造方法。 - 前記溶媒の粘性率は、1.66mPa・s以下である、
請求項6に記載の分離膜構造体の製造方法。 - 前記溶媒は、水及びエタノールの少なくとも一方を含む、
請求項6又は7に記載の分離膜構造体の製造方法。 - 前記溶液を乾燥させる工程において、前記貫通孔内の風速を1.0m/s以上とする、
請求項5乃至8のいずれかに記載の分離膜構造体の製造方法。
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JP2010110704A (ja) * | 2008-11-07 | 2010-05-20 | Ngk Insulators Ltd | 分離膜の製造方法 |
JPWO2010070992A1 (ja) * | 2008-12-19 | 2012-05-24 | 日本碍子株式会社 | 液体混合物の分離方法、及び液体混合物分離装置 |
CN102348494B (zh) * | 2009-03-16 | 2014-09-17 | 日本碍子株式会社 | 沸石分离膜构件、其制造方法、混合流体的分离方法以及混合流体分离装置 |
US8101010B2 (en) * | 2009-05-28 | 2012-01-24 | Corning Incorporated | Gas separation module |
WO2011004660A1 (ja) * | 2009-07-10 | 2011-01-13 | 日本碍子株式会社 | 炭素膜の製造方法、炭素膜、及び分離装置 |
EP2540384B1 (en) * | 2010-02-25 | 2022-02-16 | NGK Insulators, Ltd. | Process for producing zeolite film |
JP2012040549A (ja) * | 2010-07-22 | 2012-03-01 | Ngk Insulators Ltd | シリカ膜、及びその製造方法 |
WO2012128217A1 (ja) * | 2011-03-22 | 2012-09-27 | 日本碍子株式会社 | ハニカム形状セラミック製分離膜構造体 |
CA2851219A1 (en) | 2011-10-11 | 2013-04-18 | Ngk Insulators, Ltd. | Ceramic filter with glass seals having clay particles dispersed therein |
WO2013136869A1 (ja) * | 2012-03-16 | 2013-09-19 | 日本碍子株式会社 | 分離膜の製造方法、分離膜複合体の製造方法、及び分離膜複合体 |
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