JP2015501716A - コージエライトモノリスにコーティングされたコージエライト系複合膜 - Google Patents
コージエライトモノリスにコーティングされたコージエライト系複合膜 Download PDFInfo
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- JP2015501716A JP2015501716A JP2014541132A JP2014541132A JP2015501716A JP 2015501716 A JP2015501716 A JP 2015501716A JP 2014541132 A JP2014541132 A JP 2014541132A JP 2014541132 A JP2014541132 A JP 2014541132A JP 2015501716 A JP2015501716 A JP 2015501716A
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- Prior art keywords
- cordierite
- ceramic
- monolith
- slip
- particles
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- 229910052878 cordierite Inorganic materials 0.000 title claims abstract description 318
- 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 title claims abstract description 317
- 239000002131 composite material Substances 0.000 title claims abstract description 240
- 239000012528 membrane Substances 0.000 title claims abstract description 237
- 239000000919 ceramic Substances 0.000 claims abstract description 274
- 239000002245 particle Substances 0.000 claims abstract description 221
- 239000011148 porous material Substances 0.000 claims abstract description 106
- 238000010304 firing Methods 0.000 claims abstract description 23
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 71
- 238000000034 method Methods 0.000 claims description 51
- 239000000203 mixture Substances 0.000 claims description 32
- 238000002156 mixing Methods 0.000 claims description 19
- 239000002518 antifoaming agent Substances 0.000 claims description 13
- 239000002270 dispersing agent Substances 0.000 claims description 13
- 239000003795 chemical substances by application Substances 0.000 claims description 9
- 239000011230 binding agent Substances 0.000 claims description 8
- 238000000227 grinding Methods 0.000 claims description 7
- 239000010408 film Substances 0.000 description 37
- 239000000758 substrate Substances 0.000 description 34
- 238000000576 coating method Methods 0.000 description 32
- 239000011248 coating agent Substances 0.000 description 24
- 238000009826 distribution Methods 0.000 description 18
- 239000000463 material Substances 0.000 description 17
- 229920000642 polymer Polymers 0.000 description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 14
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 10
- 239000010410 layer Substances 0.000 description 10
- 239000007787 solid Substances 0.000 description 10
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 8
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 8
- 239000000839 emulsion Substances 0.000 description 8
- 239000002202 Polyethylene glycol Substances 0.000 description 7
- ISWQCIVKKSOKNN-UHFFFAOYSA-L Tiron Chemical group [Na+].[Na+].OC1=CC(S([O-])(=O)=O)=CC(S([O-])(=O)=O)=C1O ISWQCIVKKSOKNN-UHFFFAOYSA-L 0.000 description 7
- 229910010293 ceramic material Inorganic materials 0.000 description 7
- 229920001223 polyethylene glycol Polymers 0.000 description 7
- 229920005596 polymer binder Polymers 0.000 description 7
- 239000002491 polymer binding agent Substances 0.000 description 7
- 239000000843 powder Substances 0.000 description 7
- 238000002360 preparation method Methods 0.000 description 7
- 239000000243 solution Substances 0.000 description 7
- 238000001035 drying Methods 0.000 description 6
- 238000010438 heat treatment Methods 0.000 description 6
- 239000003973 paint Substances 0.000 description 6
- 238000000926 separation method Methods 0.000 description 6
- 238000000498 ball milling Methods 0.000 description 5
- 238000003801 milling Methods 0.000 description 5
- 239000003960 organic solvent Substances 0.000 description 5
- 239000000377 silicon dioxide Substances 0.000 description 5
- 229910021536 Zeolite Inorganic materials 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 4
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 description 4
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 description 4
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 4
- 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 4
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 4
- 229910052753 mercury Inorganic materials 0.000 description 4
- 229910052863 mullite Inorganic materials 0.000 description 4
- 238000001878 scanning electron micrograph Methods 0.000 description 4
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 4
- 229910010271 silicon carbide Inorganic materials 0.000 description 4
- 229910001233 yttria-stabilized zirconia Inorganic materials 0.000 description 4
- RUDFQVOCFDJEEF-UHFFFAOYSA-N yttrium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Y+3].[Y+3] RUDFQVOCFDJEEF-UHFFFAOYSA-N 0.000 description 4
- 239000010457 zeolite Substances 0.000 description 4
- 229910052581 Si3N4 Inorganic materials 0.000 description 3
- 238000001354 calcination Methods 0.000 description 3
- 238000001914 filtration Methods 0.000 description 3
- 239000011521 glass Substances 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 3
- 239000002002 slurry Substances 0.000 description 3
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 3
- 229910001887 tin oxide Inorganic materials 0.000 description 3
- 239000004372 Polyvinyl alcohol Substances 0.000 description 2
- 239000003125 aqueous solvent Substances 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 230000003247 decreasing effect Effects 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- 239000006260 foam Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000011236 particulate material Substances 0.000 description 2
- 230000000704 physical effect Effects 0.000 description 2
- 229920003023 plastic Polymers 0.000 description 2
- 239000004033 plastic Substances 0.000 description 2
- 229920006254 polymer film Polymers 0.000 description 2
- 229920002451 polyvinyl alcohol Polymers 0.000 description 2
- 230000003746 surface roughness Effects 0.000 description 2
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- SNAAJJQQZSMGQD-UHFFFAOYSA-N aluminum magnesium Chemical compound [Mg].[Al] SNAAJJQQZSMGQD-UHFFFAOYSA-N 0.000 description 1
- 239000011324 bead Substances 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 239000013530 defoamer Substances 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 210000004709 eyebrow Anatomy 0.000 description 1
- 238000010097 foam moulding Methods 0.000 description 1
- 229920001002 functional polymer Polymers 0.000 description 1
- 239000008240 homogeneous mixture Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 238000003760 magnetic stirring Methods 0.000 description 1
- 238000005121 nitriding Methods 0.000 description 1
- 238000000643 oven drying Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000013618 particulate matter Substances 0.000 description 1
- 229910052573 porcelain Inorganic materials 0.000 description 1
- 238000002459 porosimetry Methods 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 238000005549 size reduction Methods 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
- 238000001238 wet grinding Methods 0.000 description 1
Classifications
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- Y10T428/24—Structurally defined web or sheet [e.g., overall dimension, etc.]
- Y10T428/24149—Honeycomb-like
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- Materials Engineering (AREA)
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- Chemical Kinetics & Catalysis (AREA)
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- Nanotechnology (AREA)
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Abstract
Description
(Mg,Fe)2Al3(Si5AlO18)
による組成物を有する固溶体である。本明細書における実施形態によると、コージエライトモノリスを形成するために使用されるコージエライト材料の的確な組成物は変更されてもよい。例えば、マグネシウム、アルミニウムおよびシリカ原料の粒径の変更により、コージエライト材料の孔径は制御されてもよく、コージエライトの細孔率は制御されてもよく、また、コージエライト材料の細孔径分布は、制御されてもよい。さらに、細孔形成剤がコージエライトモノリスを形成するために使用されるコージエライトバッチに包含されてもよい。
2.5μmのコージエライト−アルミナ複合スリップの調製
この実施例は、平均粒度2.5μmを有するコージエライト原料とアルミナ原料との異なる重量比を使用する、2つのコージエライト−アルミナ複合スリップの調製について記述する。コージエライトは、最初のメジアン粒径(d50)が11.6μmである市販の粉砕されたコージエライト原料で、アルミナは最初のd50が0.2〜0.3μmであるA−16であった。2つのうちの1つ目のスリップにおけるコージエライトのアルミナに対する比率は、7:3であり、2つのうちの2つ目のスリップにおけるコージエライトのアルミナに対する比率は、3:7であった。
1.0μmのコージエライト−アルミナ複合スリップの調製
この実施例は、平均粒度1.0μmを有するコージエライト原料とアルミナ原料との異なる重量比を使用する、2つのコージエライト−アルミナ複合スリップの調製について記述する。この実施例において使用されるコージエライトは、最初のd50が約2μmである微細なコージエライト原料で、アルミナは最初のd50が0.2〜0.3μmであるA−16であった。2つのうちの1つ目のスリップにおけるコージエライトのアルミナに対する比率は、7:3であり、2つのうちの2つ目のスリップにおけるコージエライトのアルミナに対する比率は、3:7であった。
支持されていない2.5μmのコージエライト−アルミナ複合膜
この実施例は、2つの支持されていない、コージエライト−アルミナ複合スリップの調製について記述する。1つ目は、コージエライト70重量%の2.5μmコージエライト−アルミナ複合膜であり、2つ目は、コージエライト30重量%の2.5μmコージエライト−アルミナ複合膜である。複合膜は、実施例1に記述された対応するスリップを使用して、濾紙へのスリップコーティングにより作られ、続いて乾燥と焼成が行われた。
支持されていない1.0μmコージエライト−アルミナ複合膜
この実施例は、2つの追加の支持されていないコージエライト−アルミナ複合膜の調製について記述する。1つ目は、コージエライト70重量%の1μmコージエライト−アルミナ複合膜であり、2つ目はコージエライト30重量%の1μmコージエライト−アルミナ複合膜である。複合膜は、実施例2に記述された対応するスリップを使用して、濾紙へのスリップコーティングにより作られ、続いて乾燥と焼成が行われた。
コージエライトモノリス基材に堆積させたコージエライト−アルミナ複合膜
この実施例は、モノリスコージエライト基材上にコーティングされたコージエライト−アルミナ複合膜について記述する。この実施例において使用するモノリスコージエライト基材は、外径1インチ(2.74cm)および長さ2インチ(5.48cm)を有するコージエライトからなり、断面積にわたり均一に分散された、平均直径1.8mmの91本の丸いチャネルを含む。水銀ポロシメーターにより測定されたように、モノリス基材は4.4μmのメジアン孔径および46〜47%の細孔率を有した。基材はチャネルを通してDI水でフラッシングし、オーブンにおいて120℃で一晩完全に乾燥した。
膜コーティング性
本実施例では、粒の粗いコージエライト粒子を細かいアルミナ粒子と混合する影響について記述し、以下のポリマーコーティングの孔隙構造およびコーティング性については実施例1〜5を通して説明した通りである。コージエライトのみの膜は、実施例5において使用された1インチ×2インチ(2.74cm×5.48cm)と同じタイプのコージエライトモノリス基材上の2.5μmコージエライトスリップから作られた。コージエライト膜を、1℃/分の加熱速度、1150℃で2時間の滞留時間および−2℃/分の冷却速度を使用して焼成した。2.5μmコージエライトスリップの代わりに1.8μmコージエライトスリップを使用したこと以外は同じ手順を使用して、2つ目のコージエライトのみの膜を調製した。
Claims (5)
- 表面メジアン孔径が約1μm〜約15μmの表面を有するコージエライトモノリスと;
前記コージエライトモノリスの表面に接合された、膜面を有するコージエライト−セラミック複合膜と;
を含む複合膜モノリスであって:
前記コージエライト−セラミック複合膜が:
前記表面メジアン孔径より小さいコージエライトメジアン粒径を有するコージエライト粒子と;
前記コージエライト粒子以外の、前記コージエライトメジアン粒径より小さいセラミックメジアン粒径を有するセラミック粒子と;
を含む混合物から形成された複合体であって;
前記膜面が0.3μm以下の膜メジアン孔径を有することを特徴とする複合膜モノリス。 - 前記コージエライトメジアン粒径が約0.8μm〜約5μmであり、前記セラミックメジアン粒径が約0.05μm〜約0.5μmであることを特徴とする、請求項1に記載の複合膜モノリス。
- 前記セラミック粒子がアルミナ粒子であることを特徴とする、請求項1または2の複合膜モノリス。
- コージエライトモノリスの表面にコージエライト−セラミック複合スリップを適用するステップであって、前記コージエライト−セラミック複合スリップが、コーティングされたコージエライトモノリスを形成するためのコージエライト粒子およびコージエライト粒子以外にセラミック粒子を含み、前記モノリスの表面が、約1μm〜約15μmの表面メジアン孔径を有し、前記コージエライト粒子が、表面メジアン孔径より小さいコージエライトメジアン粒径を有し、前記セラミック粒子が、前記コージエライトメジアン粒径より小さいセラミックメジアン粒径を有し、前記コージエライト−セラミックス複合スリップが、前記コージエライト粒子と前記セラミック粒子の総合重量に基づいて、30重量%〜90の重量%のコージエライト粒子および10重量%〜70の重量%のセラミック粒子を含み、前記コージエライトメジアン粒径が約0.8μm〜約5μmで、前記セラミックメジアン粒径が約0.05μm〜約0.5μmであるステップと;
前記コーティングされたコージエライトモノリスを焼成し、複合膜モノリスを形成するステップであって、焼成中に、前記コージエライト−セラミック複合スリップが、前記コージエライトモノリスの表面に接合され、かつ、0.3μm以下の膜メジアン孔径を有する膜面を有する、コージエライト−セラミック複合膜を形成するステップと;
を含むことを特徴とする、複合膜モノリスを形成する方法。 - コージエライトスリップとセラミックスリップを混合し、コージエライト−セラミック複合スリップを形成するステップをさらに含み:
前記コージエライト粒子をビヒクル、粉砕媒体、ならびに、結合剤、分散剤および消泡剤から成る群から選択された少なくとも1つの成分と混合し、コージエライト混合物を形成するステップと;
その中の前記コージエライト粒子が前記コージエライトモノリスの表面メジアン孔径未満のメジアン粒径になるまで、前記コージエライト混合物を粉砕し、前記コージエライトスリップを形成するステップと;
により、前記コージエライトスリップを形成することを特徴とする、請求項4に記載の方法。
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