JP5747127B2 - アルミナ多孔質体およびその製造方法 - Google Patents
アルミナ多孔質体およびその製造方法 Download PDFInfo
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- JP5747127B2 JP5747127B2 JP2014521219A JP2014521219A JP5747127B2 JP 5747127 B2 JP5747127 B2 JP 5747127B2 JP 2014521219 A JP2014521219 A JP 2014521219A JP 2014521219 A JP2014521219 A JP 2014521219A JP 5747127 B2 JP5747127 B2 JP 5747127B2
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- alumina
- porous body
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- rare earth
- ceramic
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- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 title claims description 313
- 238000004519 manufacturing process Methods 0.000 title claims description 37
- 239000002245 particle Substances 0.000 claims description 120
- 239000000919 ceramic Substances 0.000 claims description 68
- 238000002156 mixing Methods 0.000 claims description 64
- 238000010304 firing Methods 0.000 claims description 46
- 229910001404 rare earth metal oxide Inorganic materials 0.000 claims description 39
- 239000002002 slurry Substances 0.000 claims description 39
- 229910052622 kaolinite Inorganic materials 0.000 claims description 35
- 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 claims description 33
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 claims description 33
- 229910052863 mullite Inorganic materials 0.000 claims description 33
- 238000000465 moulding Methods 0.000 claims description 27
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 claims description 25
- 238000000034 method Methods 0.000 claims description 22
- 229910052604 silicate mineral Inorganic materials 0.000 claims description 21
- 239000012528 membrane Substances 0.000 claims description 17
- 150000001875 compounds Chemical class 0.000 claims description 16
- 239000000843 powder Substances 0.000 claims description 15
- 229910021193 La 2 O 3 Inorganic materials 0.000 claims description 14
- 239000000463 material Substances 0.000 claims description 11
- 229910052688 Gadolinium Inorganic materials 0.000 claims description 8
- UIWYJDYFSGRHKR-UHFFFAOYSA-N gadolinium atom Chemical compound [Gd] UIWYJDYFSGRHKR-UHFFFAOYSA-N 0.000 claims description 8
- 229910052746 lanthanum Inorganic materials 0.000 claims description 8
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 claims description 8
- 238000007581 slurry coating method Methods 0.000 claims description 8
- 229910052727 yttrium Inorganic materials 0.000 claims description 8
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- 239000011230 binding agent Substances 0.000 claims description 6
- 238000002844 melting Methods 0.000 claims description 6
- 230000008018 melting Effects 0.000 claims description 6
- 238000001354 calcination Methods 0.000 claims 3
- 230000000052 comparative effect Effects 0.000 description 49
- 239000011148 porous material Substances 0.000 description 40
- 239000010408 film Substances 0.000 description 38
- RUDFQVOCFDJEEF-UHFFFAOYSA-N yttrium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Y+3].[Y+3] RUDFQVOCFDJEEF-UHFFFAOYSA-N 0.000 description 37
- 238000001878 scanning electron micrograph Methods 0.000 description 35
- LNUFLCYMSVYYNW-ZPJMAFJPSA-N [(2r,3r,4s,5r,6r)-2-[(2r,3r,4s,5r,6r)-6-[(2r,3r,4s,5r,6r)-6-[(2r,3r,4s,5r,6r)-6-[[(3s,5s,8r,9s,10s,13r,14s,17r)-10,13-dimethyl-17-[(2r)-6-methylheptan-2-yl]-2,3,4,5,6,7,8,9,11,12,14,15,16,17-tetradecahydro-1h-cyclopenta[a]phenanthren-3-yl]oxy]-4,5-disulfo Chemical compound O([C@@H]1[C@@H](COS(O)(=O)=O)O[C@@H]([C@@H]([C@H]1OS(O)(=O)=O)OS(O)(=O)=O)O[C@@H]1[C@@H](COS(O)(=O)=O)O[C@@H]([C@@H]([C@H]1OS(O)(=O)=O)OS(O)(=O)=O)O[C@@H]1[C@@H](COS(O)(=O)=O)O[C@H]([C@@H]([C@H]1OS(O)(=O)=O)OS(O)(=O)=O)O[C@@H]1C[C@@H]2CC[C@H]3[C@@H]4CC[C@@H]([C@]4(CC[C@@H]3[C@@]2(C)CC1)C)[C@H](C)CCCC(C)C)[C@H]1O[C@H](COS(O)(=O)=O)[C@@H](OS(O)(=O)=O)[C@H](OS(O)(=O)=O)[C@H]1OS(O)(=O)=O LNUFLCYMSVYYNW-ZPJMAFJPSA-N 0.000 description 13
- 238000005245 sintering Methods 0.000 description 12
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- WWTBZEKOSBFBEM-SPWPXUSOSA-N (2s)-2-[[2-benzyl-3-[hydroxy-[(1r)-2-phenyl-1-(phenylmethoxycarbonylamino)ethyl]phosphoryl]propanoyl]amino]-3-(1h-indol-3-yl)propanoic acid Chemical compound N([C@@H](CC=1C2=CC=CC=C2NC=1)C(=O)O)C(=O)C(CP(O)(=O)[C@H](CC=1C=CC=CC=1)NC(=O)OCC=1C=CC=CC=1)CC1=CC=CC=C1 WWTBZEKOSBFBEM-SPWPXUSOSA-N 0.000 description 10
- 238000001035 drying Methods 0.000 description 10
- 238000002474 experimental method Methods 0.000 description 10
- 239000002210 silicon-based material Substances 0.000 description 10
- 229940126208 compound 22 Drugs 0.000 description 9
- 238000007598 dipping method Methods 0.000 description 7
- 239000011521 glass Substances 0.000 description 7
- 239000012530 fluid Substances 0.000 description 6
- 238000000280 densification Methods 0.000 description 5
- 238000010586 diagram Methods 0.000 description 5
- 238000004898 kneading Methods 0.000 description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- -1 Gd 2 O 3 Inorganic materials 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 238000005266 casting Methods 0.000 description 3
- 238000001914 filtration Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 238000000634 powder X-ray diffraction Methods 0.000 description 3
- 239000010409 thin film Substances 0.000 description 3
- 229910021536 Zeolite Inorganic materials 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 229910001649 dickite Inorganic materials 0.000 description 2
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 2
- 238000001125 extrusion Methods 0.000 description 2
- 229910052621 halloysite Inorganic materials 0.000 description 2
- 239000011812 mixed powder Substances 0.000 description 2
- 229910052761 rare earth metal Inorganic materials 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000000790 scattering method Methods 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- 239000010457 zeolite Substances 0.000 description 2
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 229940125810 compound 20 Drugs 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- JAXFJECJQZDFJS-XHEPKHHKSA-N gtpl8555 Chemical compound OC(=O)C[C@H](N)C(=O)N[C@@H](CCC(O)=O)C(=O)N[C@@H](C(C)C)C(=O)N[C@@H](C(C)C)C(=O)N1CCC[C@@H]1C(=O)N[C@H](B1O[C@@]2(C)[C@H]3C[C@H](C3(C)C)C[C@H]2O1)CCC1=CC=C(F)C=C1 JAXFJECJQZDFJS-XHEPKHHKSA-N 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 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
- 229920000609 methyl cellulose Polymers 0.000 description 1
- 239000001923 methylcellulose Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- VXPLXMJHHKHSOA-UHFFFAOYSA-N propham Chemical compound CC(C)OC(=O)NC1=CC=CC=C1 VXPLXMJHHKHSOA-UHFFFAOYSA-N 0.000 description 1
- 150000002910 rare earth metals Chemical class 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
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Description
ここで実験Iを説明する。図2の製造工程P1〜P5において、図3に示すように、第1混合工程P1における粗粒アルミナに添加されるムライトの添加量を0.00(mol%)〜2.82(mol%)の範囲内すなわち0.00(mol%)、0.28(mol%)、0.85(mol%)、1.42(mol%)、1.99(mol%)、2.39(mol%)、2.53(mol%)、2.82(mol%)に変化させ、第1混合工程P1における粗粒アルミナに添加されるイットリアの添加量を0.00(mol%)〜2.82(mol%)の範囲内すなわち0.00(mol%)、0.29(mol%)、0.45(mol%)、0.85(mol%)、1.42(mol%)、1.99(mol%)、2.56(mol%)、2.82(mol%)に変化させることによって、8種類の試料であるアルミナ多孔質体10すなわち実施例品1〜3、比較例品1〜5のアルミナ多孔質体10を製造し、それらアルミナ多孔質体10の平均圧環強度KA(MPa)、平均細孔径(μm)、気孔率(%)を測定すると共に、それらアルミナ多孔質体10内のネックの主成分を調べた。なお、前記ネックとは、アルミナ多孔質体10内において骨材であるアルミナ粒子16の間のボンドである。
圧環強度K(MPa)=(F×(D−e))/(L×e2)・・・(1)
ここで実験IIを説明する。図2の製造工程P1〜P5において、図15に示すように、第1混合工程P1におけるアルミナに添加されるカオリナイトの添加量を0.44(mol%)〜4.40(mol%)の範囲内すなわち0.44(mol%)、1.32(mol%)、2.20(mol%)、3.08(mol%)、3.46(mol%)、3.70(mol%)、3.83(mol%)、3.95(mol%)、4.40(mol%)に変化させ、第1混合工程P1におけるアルミナに添加されるイットリアの添加量を0.00(mol%)〜3.96(mol%)の範囲内すなわち0.00(mol%)、0.45(mol%)、0.57(mol%)、0.70(mol%)、0.95(mol%)、1.32(mol%)、2.20(mol%)、3.08(mol%)、3.96(mol%)に変化させることによって、9種類の試料であるアルミナ多孔質体10すなわち実施例品4〜8、比較例品6〜9のアルミナ多孔質体10を製造し、それらアルミナ多孔質体10の平均圧環強度KA(MPa)、平均細孔径(μm)、気孔率(%)を測定すると共に、それらアルミナ多孔質体10内のネックの主成分を調べた。
ここで実験IIIを説明する。図30の製造工程P1〜P9において第1混合工程P1におけるアルミナに添加されるムライトの添加量を1.99mol%にし、第1混合工程P1におけるアルミナに添加されるイットリアの添加量を0.85mol%にして、実施例2の二層構造のセラミック多孔質体14を製造した。また、パイプ状グリーン成形体を1450℃で2時間焼成させた実施例品2のアルミナ多孔質体10を第2混合工程P6によって調整されたスラリーをディッピングして乾燥させた後、再度1450℃で2時間焼成して比較例の二層構造のセラミック多孔質体14を製造した。そして、これら二層構造のセラミック多孔質体14の無機多孔質膜12の状態を図31および図32を用いて比較した。なお、図31は実施例2の二層構造のセラミック多孔質体14の破断面の一部を走査型電子顕微鏡により撮影したSEM像であり、図32は比較例の二層構造のセラミック多孔質体14の無機多孔質膜12の表面の一部を走査型電子顕微鏡により撮影したSEM像である。
12:無機多孔質膜
12a:無機粉末
14:二層構造のセラミック多孔質体
16:アルミナ粒子
18:Si系化合物
20:希土類酸化物
22:化合物
P1:第1混合工程
P3:成形工程
P6:第2混合工程
P7:ディッピング工程(スラリーコーティング工程)
P5、P9:焼成工程
Claims (9)
- 骨材であるアルミナ粒子間を結合することで構成され、前記骨材のアルミナ粒子間は、ケイ酸塩鉱物とGd2O3、La2O3、Y2O3から選ばれた少なくとも1種類の希土類酸化物とから合成される、ケイ酸ガドリニウム、ケイ酸ランタン、またはケイ酸イットリウムから成る化合物にて結合されているアルミナ多孔質体と、
該アルミナ多孔質体上に形成された無機多孔質膜と
を、有することを特徴とするセラミック多孔質体。 - 前記ケイ酸塩鉱物としてムライトを、前記希土類酸化物としてY2O3を用いて、それ等のモル比が0.5〜7.5の範囲内となるように混合するものである請求項1のセラミック多孔質体。
- 前記ケイ酸塩鉱物としてカオリナイトを、前記希土類酸化物としてY2O3を用いて、それ等のモル比が0.2〜6.2の範囲内となるように混合するものである請求項1のセラミック多孔質体。
- 請求項1のアルミナ多孔質体の製造方法であって、
骨材のアルミナ粒子に、ケイ酸塩鉱物とGd2O3、La2O3、Y2O3から選ばれた少なくとも1種類の希土類酸化物とを混合する第1混合工程と、
前記第1混合工程によって混合された材料から所定形状に成形する成形工程と、
前記成形工程によって成形された成形体を、前記化合物が合成され且つその溶融によって前記アルミナ粒子間を結合する焼成温度で焼成する焼成工程と
を含むアルミナ多孔質体の製造方法。 - 前記第1混合工程は、前記ケイ酸塩鉱物としてムライトを、前記希土類酸化物としてY2O3を用いて、それ等のモル比が0.5〜7.5の範囲内となるように混合するものである請求項4のアルミナ多孔質体の製造方法。
- 前記第1混合工程は、前記ケイ酸塩鉱物としてカオリナイトを、前記希土類酸化物としてY2O3を用いて、それ等のモル比が0.2〜6.2の範囲内となるように混合するものである請求項4のアルミナ多孔質体の製造方法。
- 請求項1のアルミナ多孔質体上に無機多孔質膜を形成する二層構造のセラミック多孔質体の製造方法であって、
骨材のアルミナ粒子に、ケイ酸塩鉱物とGd2O3、La2O3、Y2O3から選ばれた少なくとも1種類の希土類酸化物とを混合する第1混合工程と、
前記第1混合工程によって混合された材料から所定形状に成形する成形工程と、
前記無機多孔質膜を構成する無機粉末に有機バインダーおよび水を混合させてスラリーを調整する第2混合工程と、
前記成形工程によって成形された成形体の表面に前記第2混合工程によって調整されたスラリーを層状に付着させるスラリーコーティング工程と、
前記スラリーコーティング工程によってスラリーが層状に付着した成形体を、前記化合物が合成され且つその溶融によって前記アルミナ粒子間を結合する焼成温度で焼成する焼成工程と
を含むアルミナ多孔質体上に無機多孔質膜を形成する二層構造のセラミック多孔質体の製造方法。 - 前記第1混合工程は、前記ケイ酸塩鉱物としてムライトを、前記希土類酸化物としてY2O3を用いて、それ等のモル比が0.5〜7.5の範囲内となるように混合するものである請求項7のアルミナ多孔質体上に無機多孔質膜を形成する二層構造のセラミック多孔質体の製造方法。
- 前記第1混合工程は、前記ケイ酸塩鉱物としてカオリナイトを、前記希土類酸化物としてY2O3を用いて、それ等のモル比が0.2〜6.2の範囲内となるように混合するものである請求項7のアルミナ多孔質体上に無機多孔質膜を形成する二層構造のセラミック多孔質体の製造方法。
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US4757045A (en) * | 1983-02-14 | 1988-07-12 | Engelhard Corporation | Catalysts with support coatings having increased macroporosity and method for producing the catalysts |
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