JPWO2016158583A1 - ゼオライト膜構造体及びその製造方法 - Google Patents
ゼオライト膜構造体及びその製造方法 Download PDFInfo
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- 229910021536 Zeolite Inorganic materials 0.000 title claims abstract description 122
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 title claims abstract description 122
- 239000010457 zeolite Substances 0.000 title claims abstract description 122
- 239000012528 membrane Substances 0.000 title claims abstract description 58
- 238000004519 manufacturing process Methods 0.000 title claims description 10
- 239000011148 porous material Substances 0.000 claims abstract description 47
- 239000013078 crystal Substances 0.000 claims description 41
- 230000001186 cumulative effect Effects 0.000 claims description 16
- 239000002245 particle Substances 0.000 claims description 16
- 239000002002 slurry Substances 0.000 claims description 11
- 238000010899 nucleation Methods 0.000 claims description 7
- 238000000790 scattering method Methods 0.000 claims description 4
- 239000010410 layer Substances 0.000 description 106
- 239000002344 surface layer Substances 0.000 description 46
- 239000002585 base Substances 0.000 description 15
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 14
- 239000000243 solution Substances 0.000 description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 13
- 239000002994 raw material Substances 0.000 description 11
- 238000000926 separation method Methods 0.000 description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 8
- DKNWSYNQZKUICI-UHFFFAOYSA-N amantadine Chemical compound C1C(C2)CC3CC2CC1(N)C3 DKNWSYNQZKUICI-UHFFFAOYSA-N 0.000 description 8
- 238000010438 heat treatment Methods 0.000 description 8
- 238000000034 method Methods 0.000 description 8
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 6
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 6
- 239000000377 silicon dioxide Substances 0.000 description 6
- 239000000758 substrate Substances 0.000 description 6
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 description 5
- 239000011230 binding agent Substances 0.000 description 5
- 230000004907 flux Effects 0.000 description 5
- 238000005259 measurement Methods 0.000 description 5
- 230000035699 permeability Effects 0.000 description 5
- -1 polyethylene Polymers 0.000 description 5
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- 210000004027 cell Anatomy 0.000 description 4
- 239000006185 dispersion Substances 0.000 description 4
- 238000001027 hydrothermal synthesis Methods 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 238000009792 diffusion process Methods 0.000 description 3
- 238000001914 filtration Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 239000012466 permeate Substances 0.000 description 3
- 229910001220 stainless steel Inorganic materials 0.000 description 3
- 239000010935 stainless steel Substances 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 239000004927 clay Substances 0.000 description 2
- 239000000470 constituent Substances 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
- 239000011521 glass Substances 0.000 description 2
- 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 2
- 239000007788 liquid Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 238000000465 moulding Methods 0.000 description 2
- 229910052863 mullite Inorganic materials 0.000 description 2
- 229920000620 organic polymer Polymers 0.000 description 2
- 239000003002 pH adjusting agent Substances 0.000 description 2
- 230000002093 peripheral effect Effects 0.000 description 2
- 229920001721 polyimide Polymers 0.000 description 2
- 239000004094 surface-active agent Substances 0.000 description 2
- 238000002834 transmittance Methods 0.000 description 2
- GHOKWGTUZJEAQD-ZETCQYMHSA-N (D)-(+)-Pantothenic acid Chemical compound OCC(C)(C)[C@@H](O)C(=O)NCCC(O)=O GHOKWGTUZJEAQD-ZETCQYMHSA-N 0.000 description 1
- 238000012935 Averaging Methods 0.000 description 1
- 229910000906 Bronze Inorganic materials 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
- 239000004642 Polyimide Substances 0.000 description 1
- 239000004743 Polypropylene Substances 0.000 description 1
- 229910052581 Si3N4 Inorganic materials 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- 229910000971 Silver steel Inorganic materials 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 239000012670 alkaline solution Substances 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000012298 atmosphere Substances 0.000 description 1
- 239000011324 bead Substances 0.000 description 1
- 239000010974 bronze Substances 0.000 description 1
- 210000002421 cell wall Anatomy 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000002734 clay mineral Substances 0.000 description 1
- 239000011362 coarse particle Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- KUNSUQLRTQLHQQ-UHFFFAOYSA-N copper tin Chemical compound [Cu].[Sn] KUNSUQLRTQLHQQ-UHFFFAOYSA-N 0.000 description 1
- 229910052878 cordierite Inorganic materials 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 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 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 238000002296 dynamic light scattering Methods 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 239000012527 feed solution Substances 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- RVZRBWKZFJCCIB-UHFFFAOYSA-N perfluorotributylamine Chemical compound FC(F)(F)C(F)(F)C(F)(F)C(F)(F)N(C(F)(F)C(F)(F)C(F)(F)C(F)(F)F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)F RVZRBWKZFJCCIB-UHFFFAOYSA-N 0.000 description 1
- 229920002492 poly(sulfone) Polymers 0.000 description 1
- 229920000573 polyethylene 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
- 239000000843 powder Substances 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 1
- 229920006268 silicone film Polymers 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 239000002562 thickening agent Substances 0.000 description 1
- RUDFQVOCFDJEEF-UHFFFAOYSA-N yttrium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Y+3].[Y+3] RUDFQVOCFDJEEF-UHFFFAOYSA-N 0.000 description 1
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Abstract
Description
図1は、分離膜構造体10の構成を示す断面図である。分離膜構造体10は、多孔質支持体20とゼオライト膜30を備える。
分離膜構造体10の製造方法について説明する。
上記実施形態において、多孔質支持体20は、基体21と中間層22と表層23を有することとしたが、中間層22と表層23の一方又は両方を有していなくてもよい。多孔質支持体20が表層23を有していない場合、最表層23aは中間層22に形成される。多孔質支持体20が中間層22と表層23を有していない場合、最表層23aは基体21に形成される。
まず、平均粒径50μmのアルミナ粒子100質量部に対して無機結合材20質量部を添加し、さらに、水、分散剤及び増粘剤を加えて混練することによって坏土を作製した。
各サンプルの種結晶分散液を約20mlの水に滴下して測定可能な濃度にした後、超音波で5分以上分散させることによって種結晶の懸濁液を得た。
各サンプルを弱アルカリ溶液(NaOH溶液)に浸してDDR型ゼオライト膜を溶解することによって、多孔質支持体の表層を露出させた。
各サンプルの断面をSEMで観察することによって、DDR型ゼオライト膜のうち表層の内部に入り込んだ層(第1ゼオライト層)の平均厚みと、DDR型ゼオライト膜のうち表層の外部に出ている層(第2ゼオライト層)の平均厚みを測定した。SEM画像上で均等に離れた3箇所で測定した厚みの算術平均値を平均厚みとした。
まず、エタノールを50体積%含む水溶液(以下、「供給液」という。)を50度に加熱した。
20 多孔質支持体
21 基体
22 中間層
23 表層
23a 最表層
23b 内部層
30 ゼオライト膜
31 第1ゼオライト層
32 第2ゼオライト層
Claims (5)
- 多孔質支持体と、
ゼオライト膜と、
を備え、
前記ゼオライト膜は、前記多孔質支持体の表面の内側に配置される第1ゼオライト層と、前記多孔質支持体の前記表面の外側に配置され、前記第1ゼオライト層と一体形成される第2ゼオライト層とを有し、
前記多孔質支持体は、前記第1ゼオライト層が配置される最表層を有し、
前記第1ゼオライト層の平均厚みは、5.4μm以下であり、
細孔径分布測定装置により測定される前記最表層の体積累積細孔径分布における50%径は、0.050μm以上0.150μm以下である、
ゼオライト膜構造体。 - 前記第1ゼオライト層の平均厚みの前記第2ゼオライト層の平均厚みに対する比は、2.0以下である、
請求項1に記載のゼオライト膜構造体。 - 前記第1ゼオライト層の平均厚みは、2.5μm以下である、
請求項1又は2に記載のゼオライト膜構造体。 - ゼオライト種結晶を含有する種付け用スラリーを多孔質支持体の表面に塗布する工程と、
前記ゼオライト種結晶を結晶成長させる工程と、
を備え、
細孔径分布測定装置により測定される前記多孔質支持体の体積累積細孔径分布における90%径に対する、レーザ回折散乱法により測定される前記ゼオライト種結晶の体積累積粒度分布における10%径の比は、0.5以上であり、
細孔径分布測定装置により測定される前記多孔質支持体の体積累積細孔径分布における90%径は、0.050μm以上0.180μm以下である、
ゼオライト膜構造体の製造方法。 - 前記多孔質支持体の前記90%径に対する前記ゼオライト種結晶の前記10%径の比は、1.3以上であり、
前記多孔質支持体の前記90%径は、0.080μm以下である、
請求項4に記載のゼオライト膜構造体の製造方法。
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