CN102639460A - 钛酸铝多孔结构 - Google Patents
钛酸铝多孔结构 Download PDFInfo
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- CN102639460A CN102639460A CN2010800422751A CN201080042275A CN102639460A CN 102639460 A CN102639460 A CN 102639460A CN 2010800422751 A CN2010800422751 A CN 2010800422751A CN 201080042275 A CN201080042275 A CN 201080042275A CN 102639460 A CN102639460 A CN 102639460A
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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 abstract description 3
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 title description 3
- 239000000463 material Substances 0.000 claims abstract description 35
- 239000000203 mixture Substances 0.000 claims abstract description 21
- 238000005245 sintering Methods 0.000 claims abstract description 11
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000002243 precursor Substances 0.000 claims abstract description 8
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 6
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims abstract description 6
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 5
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 5
- 229910052574 oxide ceramic Inorganic materials 0.000 claims abstract 3
- 150000001875 compounds Chemical class 0.000 claims description 56
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 41
- 239000000126 substance Substances 0.000 claims description 31
- 229910052782 aluminium Inorganic materials 0.000 claims description 22
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 16
- 239000004411 aluminium Substances 0.000 claims description 14
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 14
- 229910052742 iron Inorganic materials 0.000 claims description 14
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 13
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 claims description 10
- 229910052726 zirconium Inorganic materials 0.000 claims description 10
- 239000002245 particle Substances 0.000 claims description 9
- 239000011777 magnesium Substances 0.000 claims description 6
- 239000011148 porous material Substances 0.000 claims description 6
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 6
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 5
- 239000003054 catalyst Substances 0.000 claims description 5
- 229910052749 magnesium Inorganic materials 0.000 claims description 5
- 229910052684 Cerium Inorganic materials 0.000 claims description 4
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 4
- 230000001413 cellular effect Effects 0.000 claims description 4
- 229960001866 silicon dioxide Drugs 0.000 claims description 4
- 238000007669 thermal treatment Methods 0.000 claims description 4
- 229910052746 lanthanum Inorganic materials 0.000 claims description 3
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 claims description 3
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 3
- GEIAQOFPUVMAGM-UHFFFAOYSA-N ZrO Inorganic materials [Zr]=O GEIAQOFPUVMAGM-UHFFFAOYSA-N 0.000 claims 1
- 238000010438 heat treatment Methods 0.000 abstract description 3
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum oxide Inorganic materials [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 abstract description 2
- QDOXWKRWXJOMAK-UHFFFAOYSA-N dichromium trioxide Chemical compound O=[Cr]O[Cr]=O QDOXWKRWXJOMAK-UHFFFAOYSA-N 0.000 abstract 2
- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Chemical compound O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 abstract 2
- 229910000421 cerium(III) oxide Inorganic materials 0.000 abstract 1
- 229910052681 coesite Inorganic materials 0.000 abstract 1
- 229910052593 corundum Inorganic materials 0.000 abstract 1
- 229910052906 cristobalite Inorganic materials 0.000 abstract 1
- QZQVBEXLDFYHSR-UHFFFAOYSA-N gallium(III) oxide Inorganic materials O=[Ga]O[Ga]=O QZQVBEXLDFYHSR-UHFFFAOYSA-N 0.000 abstract 1
- CJNBYAVZURUTKZ-UHFFFAOYSA-N hafnium(IV) oxide Inorganic materials O=[Hf]=O CJNBYAVZURUTKZ-UHFFFAOYSA-N 0.000 abstract 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 abstract 1
- KTUFCUMIWABKDW-UHFFFAOYSA-N oxo(oxolanthaniooxy)lanthanum Chemical compound O=[La]O[La]=O KTUFCUMIWABKDW-UHFFFAOYSA-N 0.000 abstract 1
- 229910052682 stishovite Inorganic materials 0.000 abstract 1
- 229910052905 tridymite Inorganic materials 0.000 abstract 1
- 229910001845 yogo sapphire Inorganic materials 0.000 abstract 1
- RUDFQVOCFDJEEF-UHFFFAOYSA-N yttrium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Y+3].[Y+3] RUDFQVOCFDJEEF-UHFFFAOYSA-N 0.000 abstract 1
- 239000003795 chemical substances by application Substances 0.000 description 10
- 238000001914 filtration Methods 0.000 description 9
- 238000000034 method Methods 0.000 description 9
- 238000006243 chemical reaction Methods 0.000 description 8
- 238000002360 preparation method Methods 0.000 description 7
- 239000000523 sample Substances 0.000 description 6
- 230000015572 biosynthetic process Effects 0.000 description 5
- 239000003153 chemical reaction reagent Substances 0.000 description 5
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 5
- 229910010271 silicon carbide Inorganic materials 0.000 description 5
- 239000000919 ceramic Substances 0.000 description 4
- 238000002425 crystallisation Methods 0.000 description 4
- 230000008025 crystallization Effects 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- 229910052760 oxygen Inorganic materials 0.000 description 4
- 230000008929 regeneration Effects 0.000 description 4
- 238000011069 regeneration method Methods 0.000 description 4
- 230000003197 catalytic effect Effects 0.000 description 3
- 238000010304 firing Methods 0.000 description 3
- 239000004071 soot Substances 0.000 description 3
- 239000010936 titanium Substances 0.000 description 3
- 229910052719 titanium Inorganic materials 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 239000011230 binding agent Substances 0.000 description 2
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 description 2
- 235000019504 cigarettes Nutrition 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000004453 electron probe microanalysis Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000003921 oil Substances 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000012958 reprocessing Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 229910000789 Aluminium-silicon alloy Inorganic materials 0.000 description 1
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
- 235000008733 Citrus aurantifolia Nutrition 0.000 description 1
- 239000004902 Softening Agent Substances 0.000 description 1
- 229920002472 Starch Polymers 0.000 description 1
- 235000011941 Tilia x europaea Nutrition 0.000 description 1
- 102100031083 Uteroglobin Human genes 0.000 description 1
- 108090000203 Uteroglobin Proteins 0.000 description 1
- -1 Vilaterm Polymers 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 150000001340 alkali metals Chemical class 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 229910052788 barium Inorganic materials 0.000 description 1
- 229910052728 basic metal Inorganic materials 0.000 description 1
- 150000003818 basic metals Chemical class 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 description 1
- ZMIGMASIKSOYAM-UHFFFAOYSA-N cerium Chemical compound [Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce] ZMIGMASIKSOYAM-UHFFFAOYSA-N 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 239000002283 diesel fuel Substances 0.000 description 1
- 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 1
- 238000007598 dipping method Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000010433 feldspar Substances 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 229910052735 hafnium Inorganic materials 0.000 description 1
- VBJZVLUMGGDVMO-UHFFFAOYSA-N hafnium atom Chemical compound [Hf] VBJZVLUMGGDVMO-UHFFFAOYSA-N 0.000 description 1
- 229910000449 hafnium oxide Inorganic materials 0.000 description 1
- WIHZLLGSGQNAGK-UHFFFAOYSA-N hafnium(4+);oxygen(2-) Chemical compound [O-2].[O-2].[Hf+4] WIHZLLGSGQNAGK-UHFFFAOYSA-N 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
- 238000009434 installation Methods 0.000 description 1
- 239000004571 lime Substances 0.000 description 1
- 239000000314 lubricant 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
- 229910052863 mullite Inorganic materials 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 125000002524 organometallic group Chemical group 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 235000011837 pasties Nutrition 0.000 description 1
- 229920003229 poly(methyl methacrylate) Polymers 0.000 description 1
- 239000004926 polymethyl methacrylate Substances 0.000 description 1
- 229910052573 porcelain Inorganic materials 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000010970 precious metal Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000003746 solid phase reaction Methods 0.000 description 1
- 238000010671 solid-state reaction Methods 0.000 description 1
- 235000019698 starch Nutrition 0.000 description 1
- 239000008107 starch Substances 0.000 description 1
- 229910052712 strontium Inorganic materials 0.000 description 1
- LEDMRZGFZIAGGB-UHFFFAOYSA-L strontium carbonate Chemical compound [Sr+2].[O-]C([O-])=O LEDMRZGFZIAGGB-UHFFFAOYSA-L 0.000 description 1
- 229910000018 strontium carbonate Inorganic materials 0.000 description 1
- 239000002912 waste gas Substances 0.000 description 1
- 238000004846 x-ray emission Methods 0.000 description 1
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Abstract
本发明涉及包含氧化物陶瓷材料的多孔结构，该氧化物陶瓷材料包含，基于相应的简单氧化物：Al2O3；TiO2；至少一种选自Fe2O3、Cr2O3、MnO2、La2O3、Y2O3、Ga2O3的元素M2氧化物；至少一种选自ZrO2、Ce2O3、HfO2的元素M3氧化物；和任选的至少一种选自MgO、CoO的元素M1氧化物和任选的SiO2；所述材料通过相应的简单氧化物或者它们的前体之一的反应性烧结或者通过具有所述组成的烧结颗粒的热处理获得。
Description
本发明涉及多孔结构，如催化剂载体或者颗粒过滤器，其构成过滤和/或活性部分的材料基于钛酸铝。形成根据本发明的载体或陶瓷过滤器的基础的陶瓷材料或者主要由元素Al、Ti的氧化物构成。所述多孔结构最通常是蜂窝状结构并且特别地用于柴油类型内燃机的排气管道中。
在本说明书的后面部分中，为了方便起见并且根据在陶瓷领域的习惯，将通过参考相应的简单氧化物(例如Al2O3或TiO2)描述所述包含所述元素的氧化物。特别地，在下面说明书中，除非另外提到，所述构成根据本发明的氧化物的不同元素的比例通过参考相应简单的氧化物的重量以相对于在所描述化学组成中存在的氧化物的总量的重量百分比给出。
在本说明书的剩余部分中，将描述在可以除去在来自汽油或者柴油内燃机的废气中包含的污染物的过滤器或者催化剂载体的特定领域(本发明涉及的领域)中的应用和优点。目前，所有用于净化废气的结构通常都具有蜂窝状结构。
据已知，在它的使用期间，颗粒过滤器经受一系列的过滤(烟灰积累)和再生(烟灰去除)阶段。在过滤阶段期间，由发动机排出的烟灰颗粒被保留和沉积在过滤器内部。在再生阶段期间，烟灰颗粒在过滤器内部被烧掉以便恢复其过滤性能。因此将理解的是，构成过滤器的材料在低温和高温时的机械强度性质对于这种应用是极其重要的。同样地，该材料必须是具有足够稳定的结构以经受，尤其在在其中装备它的交通工具的整个寿命期间，可局部升高达1000℃以上的温度，尤其如果一些再生阶段控制不良的话。
目前，过滤器主要地由多孔陶瓷材料制成，最通常地由金刚砂或者堇青石制成。这种类型的金刚砂催化过滤器例如描述在专利申请EP816065、EP1142619、EP1455923或者WO2004/090294和WO2004/065088中。这种过滤器可以获得具有优异的热导率和具有孔隙度特征(特别地平均孔径和孔径分布)的化学上惰性的过滤结构，其对于过滤由内燃机产生的烟灰的应用是理想的。
然而，仍然存在一些这种材料特有的缺点：
第一个缺点与SiC的稍微高的热膨胀系数(大于3×10-6K-1)有关，这不允许制备大尺寸的整料过滤器并且最经常必须将该过滤器分割成多个使用胶合剂结合在一起的蜂窝状元件，如在专利申请EP1455923中描述的那样。经济性的第二个缺点与极其高的允许烧结(以确保该蜂窝状结构的足够的热机械强度)的烧制温度(典型地高于2100℃)有关，特别地在过滤器的连续再生阶段期间更如此。这种温度要求安装特殊设备，这显著地提高了最后获得的过滤器的成本。
另一方面，虽然由堇青石制成的过滤器是已知的并且使用很长时间了(由于它们的低成本)，然而目前已知的是，在这种结构中可能遇到问题，特别地在控制不良的再生循环期间，在其期间，过滤器可能局部地经受高于堇青石的熔点的温度。这些热点的后果可为从过滤器的效率的部分损失至在最严重的情况下它完全的破坏。而且，堇青石不具有足够的化学惰性(考虑连续的再生循环期间达到的温度)，并因此它易于反应并被来源于在该过滤阶段期间已经积累在该结构中的润滑剂、燃料或其它油的残余物的物类腐蚀，该现象还可以是该结构的性能快速退化的原因。
例如，这种缺点已经描述在专利申请WO2004/011124中，其提出用多铝红柱石(10-40重量%)增强的基于钛酸铝(60-90重量%)的过滤器以克服它们，其耐用性得到改善。
根据另一实施方案，专利申请EP1559696提出使用粉末以制备通过在1000-1700℃使铝、钛和镁的氧化物反应性烧结获得的蜂窝式过滤器。在烧结之后获得的材料呈两种相的混合物形式：假板钛矿Al2TiO5结构类型的主相，其包含钛、铝和镁，和NayK1-yAlSi3O8类型的长石次相。
然而，由申请人进行的实验已经表明在目前难于保证这种基于钛酸铝类型材料的结构的性能，特别地难于达到适合于例如使它们能直接地用于颗粒过滤器类型的高温应用中的热稳定性、热膨胀系数的值。
本发明的目的因此是提供多孔结构，其包含具有得到明显改善的如上所述性质的氧化物材料，尤其以使得它们更有利地用于制备过滤和/或催化多孔结构，典型地蜂窝状结构。
更确切地说，本发明涉及包含陶瓷材料的多孔结构，该陶瓷材料的化学组成包含，基于氧化物以重量%计：
-大于25%并低于52%的Al2O3；
-大于26%并低于55%的TiO2；
-总计低于20%的至少一种选自MgO、CoO的元素M1氧化物；
-总计大于1%并低于20%的至少一种选自Fe2O3、Cr2O3、MnO2、La2O3、Y2O3、Ga2O3的元素M2氧化物；
-总计大于1%并低于25%，甚至总计低于20%的至少一种选自ZrO2、Ce2O3、HfO2的元素M3氧化物；
-低于20%的SiO2；
所述组成具有:
-低于10%的MgO；
-大于1%并低于20%的Fe2O3；
-大于1%并低于10%的ZrO2；
所述材料通过相应的简单氧化物或者它们的前体之一的反应性烧结或者通过满足所述组成的烧结颗粒的热处理获得。
如上所述，构成该材料的氧化物的不同元素的比例在上面配方中给出，参考相应的简单氧化物的重量，以相对于在所述化学组成中存在的氧化物总量的重量%计。然而，在本发明的范围内显然的是，虽然元素M1、M2或M3在上述关系中以相应的简单氧化物形式表示(通常在固态化学中)，但是它们在根据本发明的材料中最通常以更复杂的形式存在，至少对于主要部分是如此，并且可以特别地被包括在混合氧化物中，特别地被包括在钛酸铝类型的相中。
优选地，该多孔结构由所述陶瓷材料组成。
根据本发明的所述多孔结构此外满足这样的组成(以基于在所述组成中存在的氧化物总量的mol%计)使得a’-t+2m1+m2为-6至6，其中：
- a是的Al2O3摩尔百分比；
- s是SiO2的摩尔百分比；
- a’=a-0.37×s；
- t是TiO2的摩尔百分比；
- m1是M1的一种或多种氧化物的总摩尔百分比；和
- m2是M2的一种或多种氧化物的总摩尔百分比。
优选地，Al2O3占该化学组成的大于30%。优选地，Al2O3占该化学组成的低于51%，甚至低于50%，该百分比是基于氧化物以重量计给出。
优选地，TiO2占该化学组成的低于50%，或者低于45%，该百分比是基于氧化物以重量计给出。
优选地，如果存在，M1的一种或多种氧化物占该化学组成的大于1.5%，非常优选地大于2%。优选地，M1的一种或多种氧化物占该化学组成的低于6%，百分比基于氧化物是以重量计给出。
优选地，M1是Mg。
优选地，M2的一种或多种氧化物占该化学组成的大于1.5%，非常优选地大于2%，甚至大于3%。优选地，M2的一种或多种氧化物总计占该化学组成的低于20%，非常优选地低于15%，百分比是以重量计基于氧化物给出。
优选地，M2是Fe。作为更优选的变型，元素M2可以由铁和镧的组合构成，只要Fe2O3含量保持大于1.0%，甚至大于1.5%。
在这种实施方案中，Fe2O3(物类Fe2O3和La2O3的重量含量的总和)占该化学组成的大于1%，非常优选地大于1.5%。优选地，Fe2O3(或者Fe2O3+La2O3重量含量的总和)占该化学组成的低于20%，非常优选地低于18%，甚至低于15%，百分比是以重量计基于氧化物给出。
在一个实施方案中，该组成包含铁和镁和任选的镧。相应的氧化物Fe2O3和MgO和任选的La2O3这时按重量计并且总计占该化学组合物的化学组成的大于1%，甚至大于1.5%，非常优选地大于2%。优选地，Fe2O3和MgO和任选的La2O3共同占该化学组成的低于18%，非常优选地低于15%，百分比基于氧化物以重量计给出。
M3的一种或多种氧化物总计占该化学组成的大于1%，百分比是以重量计并基于氧化物给出。优选地，M3的一种或多种氧化物总计占该化学组成的低于10%，非常优选地低于8%。
优选地，M3仅仅是Zr。还优选的变型，元素M3可以由锆和铈的组合构成。
在上面给出的颗粒的组成中，根据本发明的其它优选实施方案，ZrO2(M3是Zr)因此可以用ZrO2和CeO2的组合替换(M3这时是Zr和Ce的组合)，只要ZrO2含量保持大于1%。
例如，在这种情况下所述材料包含按重量计大于1%并低于10%的(ZrO2+CeO2)，其中(ZrO2+CeO2)是在所述组合物中的两种氧化物的重量含量的总和。
在本说明书的范围中明显的是，该组成然而可能包括其它呈不可避免杂质形式的化合物。特别地，甚至当最初将仅仅一种包含锆的反应剂引入到制备根据本发明的结构的方法中时，已知所述反应剂最通常包括呈不可避免杂质形式的少量铪，其有时可以最高至该引入锆的总量的1mol%或2mol%。
例如，该材料可以具有下列化学组成，基于该氧化物以重量%计:大于35%并低于50%的Al2O3，大于26%并低于50%的TiO2，低于6%的MgO，大于2%并低于15%的Fe2O3，大于2%并低于8%的ZrO2，大于0.5%并低于15%的SiO2。
相对于所有存在的氧化物的重量含量，根据本发明的结构还可以包含其它低量元素。特别地，该结构可以按重量计基于相应的氧化物SiO2以0.1-20%的量包含硅。例如，SiO2占该化学组成的大于0.1%，特别地大于0.5%，甚至大于1%或大于2%，甚至大于3%，甚至大于5%。例如，SiO2占该化学组成的低于18%，特别地低于15%，甚至低于12%，甚至低于10%，所述百分比基于氧化物以重量计给出。
该多孔结构还可以包含其它元素，如硼，Ca、Sr、Na、K、Ba类型的碱金属或碱土金属，所述元素的总和量优选地按重量计低于10%，例如按重量计低于5%，甚至4%，甚至3%(基于相应的氧化物B2O3、CaO、SrO、Na2O、K2O、BaO)，相对于在所述多孔结构中存在的所有元素的对应氧化物的重量含量。每种低量元素的百分比含量，基于对应氧化物的重量，例如低于4%，甚至3%，甚至1%。
根据本发明的一个可能的实施方案，根据本发明的多孔结构具有以下化学组成(基于氧化物的重量%)：
-大于25%并低于52%的Al2O3；
-大于26%并低于55%的TiO2；
-大于1%并低于20%的Fe2O3；
-低于20%的SiO2；
-低于10%的MgO甚至低于2%的MgO；
-大于1%并低于10%的ZrO2；和
-任选的总计大于2%并低于13%的至少一种选自B2O3、CaO、Na2O、K2O、SrO、和BaO的氧化物。
在上述化学组成中，Fe2O3可以按相同比例用Fe2O3和La2O3的组合代替。
同样地，根据可以与前面实施方案组合的另一个实施方案，在上述化学组成中，ZrO2可以按相同比例用ZrO2和CeO2的组合代替。
根据本发明的另一可能的实施方案，根据本发明的多孔结构具有以下化学组成(基于氧化物以重量%计)：
-大于35%并低于51%的Al2O3，例如为38-50%的Al2O3；
-大于26%并低于45%的TiO2；
-大于1%并低于20%的Fe2O3或(Fe2O3+La2O3)组合；
-任选的大于0.1%并低于20%的SiO2；
-低于2%的MgO甚至低于1%的MgO；
-大于1%并低于10%的ZrO2；和
-任选的总计大于2%并低于13%的至少一种选自B2O3、CaO、Na2O、K2O、SrO、BaO的氧化物。
在上述化学组成中，Fe2O3可以按相同比例用Fe2O3和La2O3的组合代替。
同样地，根据可以与前一个实施方案组合的另一个实施方案，在上述化学组成中ZrO2可以按相同比例用ZrO2和CeO2的组合代替。
这种化学组成优选地具有，以重量%计基于氧化物：
- 1-18%的Fe2O3或(Fe2O3+La2O3)；
- 3-18%的SiO2；
- 1-8%的ZrO2或(ZrO2+CeO2)。
为了避免不必要地增加本说明书的负担，如上所述地，在根据本发明的材料的组成的各种优选的实施方案之间的所有根据本发明的可能组合将不再报道。然而，显然的是，在本说明书的范围内可以设想上面描述的初始的和/或优选的值和范围的所有可能的组合，并且它们应该被认为是由本申请人在本说明书的范围内进行了描述(特别地两、三种或更多种组合)。
根据本发明的多孔结构还可以主要地包含或由含钛、铝、至少一种选自M2的元素、至少一种选自M3的元素和任选的选自M1的元素的固溶体类型的氧化物相和至少一个基本上由二氧化钛TiO2和/或氧化锆ZrO2和/或二氧化铈CeO2和/或二氧化铪HfO2组成的相和任选的至少一种含硅酸盐的相构成。
优选地，根据发明的多孔结构可以主要地包含或者由含钛、铝、铁、锆和任选的镁的固溶体类型氧化物相和至少一个基本上由二氧化钛TiO2和/或氧化锆ZrO2组成的相和任选的至少一个含硅酸盐的相构成。
所述含硅酸盐的相可以按可以为该材料总重量的0至45%的比例存在。典型地，所述含硅酸盐的相主要地由二氧化硅和氧化铝构成，在含硅酸盐的相中的二氧化硅的重量比例大于34%。
根据可能的替代实施方案：
- Al2O3可以占48-54重量%；
- TiO2可以占35-48重量%，例如38-45重量%；
- Fe2O3或(Fe2O3+La2O3)可以占1-8重量%，例如2-6重量%；
- SiO2是以低于1重量%，甚至低于0.5重量%的比例存在；
- ZrO2(或ZrO2+CeO2)低于3重量%；
- MgO可以占1-8重量%，例如2-6重量%。
构成根据本发明的多孔结构的材料可以根据任何通常用于本领域中的技术获得。
根据第一种变型，构成该结构的材料可以直接地，以常规方式，通过以适当的比例简单混合初始反应剂(以获得希望的组成)，然后通过加热和固体状态反应(反应性烧结)获得。
所述反应剂可以是简单的氧化物(例如Al2O3、TiO2)，和任选地可进入该结构中的元素的其它氧化物，例如呈固溶体形式。根据本发明还可以使用所述氧化物的任何前体，例如呈以上元素的碳酸盐、氢氧化物或者其它有机金属形式。术语“前体”理解为在通常在热处理之前的阶段，即在一般地低于1000℃，甚至低于800℃甚至低于500℃的加热温度下，其分解成相应的简单氧化物的材料。
根据另一种制备根据本发明的结构的方法，所述反应剂是对应于如上所述的化学组成的并由所述简单氧化物获得的烧结颗粒。预烧结所述初始反应剂的混合物，即它被加热至可以允许简单氧化物反应以形成包含至少一种钛酸铝类型的结构的主相的烧结颗粒的温度。根据这种实施方案还可以使用上述的氧化物的前体。完全如同上述，烧结所述前体的混合物，即它被加热至可以使前体反应以便形成至少主要地包含钛酸铝类型结构的相的烧结颗粒的温度。
一种用于制备这种根据本发明的结构的方法通常为以下：
首先，将初始反应剂以适当的比例混合以获得希望的组成。
以在本领域中熟知的方式，该制备方法一般地包括使反应剂的初始混合物与甲基纤维素类型的有机粘结剂和致孔剂(例如，淀粉、石墨、聚乙烯、PMMA等等类型)混合的步骤，并且逐渐加入水直至获得可以进行挤出蜂窝状结构的步骤所需要的可塑性。
例如，在第一步期间，使初始混合物与1-30质量%的至少一种根据所希望的孔径选择的致孔剂混合，然后加入至少一种有机增塑剂和/或有机粘结剂和水。
该混合产生呈糊状物形式的均质产品。使用熟知的技术，使该产品挤出通过具有适当形状的模具的步骤可以获得蜂窝状整料。该方法然后例如可以包括干燥该获得的整料的步骤。在干燥步骤期间，获得的粗制陶瓷整料一般地通过微波干燥或者通过在足够的温度下干燥足够的时间，该温度和时间使得非化学结合水的含量为低于1质量%。在希望获得颗粒过滤器的情况下，该方法可以进一步地包括在该整料的每一端使每两个通道中一个通道阻塞的步骤。
烧制该整料(其过滤部分基于钛酸铝)的步骤原则上在高于1300℃而不超过1800℃，优选地不超过1750℃的温度下进行。该温度特别地根据存在于多孔材料中的其它相和/或氧化物进行调节。最通常，在该烧制步骤期间，整料结构在包含氧或者中性气体的气氛中被加热至1300℃-1600℃的温度。
虽然本发明的优点之一在于获得其尺寸可被大大提高的整料结构而不需要分割的可能性，与SiC过滤器(如上所述)不同，根据一个的实施方案(其然而不是优选的)，该方法可以任选地包括使用熟知的技术(例如在专利申请EP816065中描述的那些技术)将整料装配为组装过滤结构的步骤。
由根据本发明的多孔陶瓷材料制成的结构或者过滤结构优选地是蜂窝状类型。它具有大于10%，通常为20-70%，甚至30-60%的合适孔隙度，平均孔径理想地为5-60微米，特别地10-20微米，如通过水银孔率测量法使用Micromeritics 9500型设备进行测量。
这种过滤结构一般地具有包含一组通过由多孔材料形成的壁分隔的具有互相平行轴的相邻孔道或者通道的中央部分。
在颗粒过滤器中，所述孔道通过塞子在它们的一端或另一端被阻塞以便界定朝着进气口面开口的进气腔室和朝着气体排出面开口的出口腔室，使得该气体穿过该多孔壁。
本发明还涉及从如上面所述的结构并通过沉积(优选地通过浸渍)至少一个负载的或者优选地非负载的活性催化相而获得的过滤器或者催化剂载体，该活性催化相一般地包含至少一种贵金属，如Pt和/或Rh和/或Pd和任选的氧化物如CeO2、ZrO2、CeO2-ZrO2。该催化剂载体还具有蜂窝状结构，但是所述孔道不用塞子阻塞和该催化剂被沉积在该通道的孔隙中。
本发明和它的优点通过阅读以下非限制性实施例而更好地理解。在这些实施例中，除非另作说明，否则所有的百分比含量以重量计给出。
实施例
在实施例中，从以下原材料制备样品：
- Almatis CL4400FG氧化铝，其包含99.8%Al2O3的氧化铝并且具有约5.2微米的中值粒径d50；
- TRONOX T-R二氧化钛，其包含99.5%TiO2并且具有约0.3微米的直径；
- Elkem Microsilicia Grade 971U SiO2，具有99.7%的纯度；
- 具有大于98%纯度的Fe2O3；
- 包含约97% CaO的石灰，其中大于80%的颗粒具有低于80微米的直径；
- 包含大于98.5% SrCO3的碳酸锶，其由Société des Produits Chimiques Harbonnières销售；和
- 具有大于98.5%纯度和中值粒径d50=3.5微米的氧化锆，其以商标CC10由Saint-Gobain ZirPro公司销售；
- 具有大于99%纯度的氧化镧La2O3；
- 二氧化铈，包含约99% 的CeO2，具有其平均直径低于20微米的颗粒。
根据本发明的样品和对比样品从以适当的比例混合的前述反应剂获得。
更确切地说，使初始反应剂的共混物混合然后压制为圆柱形，其然后在表1中指出的温度下在空气中烧结4小时。
然后分析该制备的样品。对每个实施例样品进行的分析的结果在表1中给出。
在表1中：
1) 化学组成(以基于氧化物的重量%表示)通过X射线荧光进行测定；
2) 在耐火产品中存在的结晶相通过X射线衍射和EPMA微探针分析(电子探针微分析器)进行表征。基于如此获得的结果，能够估算每个相的重量百分比和它的组成。在表1中，AT指示钛酸铝类型的氧化物的固溶体(主相)，PS指示存在含硅酸盐的相，其它一个或多个相指示存在至少一个其它次相P2和"~"表示该相以微量形式存在；
3)存在的结晶相的稳定性通过这样的测试进行测定，所述测试在于通过X射线衍射使最初存在的结晶相与在1100℃热处理100小时之后存在的结晶相进行比较。如果反映在这种处理之后出现金刚砂Al2O3的主峰的最大强度保持低于该AT相的三个主峰的最大强度的平均值的50%，该产品被认为是稳定的，如果它保持低于30%，该产品被认为是非常稳定的(在表1中这种产品被标记为“是”)；
4) 抗压机械强度(R)在室温下在配备有10kN传送器(capteur)的LLOYD压机上通过以1mm/min的速度压缩该制备的样品进行测定；和
5) 密度通过阿基米德方法常规技术进行测量。在表1中给出的孔隙度对应于在理论密度(在没有孔隙的情况下该材料的期望的最大密度并且通过对该研磨产品的氦比重法(picnométrie hélium)进行测量)和测量密度之间的差值，其以百分比给出。
表1
从表1的数据可见孔隙度和机械强度的结合特征得到改善：对于相同的烧结温度，可见根据本发明的实施例的孔隙度与对比实施例的孔隙度是可相比的。同时，如在表1中指示，根据本发明的实施例具有比对比实施例显著更高的强度R。
因此，本发明的产品根据以下要求使得可以：
- 在施加的烧结(烧制)温度下获得较好的与该材料的希望组成有关的性质；或
- 调节该材料的高孔隙度水平(特别地通过向初始反应剂加入致孔剂)同时维持优良的机械稳定性。
Claims (12)
1.由氧化物陶瓷材料组成的多孔结构，该氧化物陶瓷材料对应于以下组成，基于氧化物以重量%计：
-大于25%并低于52%的Al2O3；
-大于26%并低于55%的TiO2；
-总计低于20%的至少一种选自MgO、CoO的元素M1氧化物；
-总计大于1%并低于20%的至少一种选自Fe2O3、Cr2O3、MnO2、La2O3、Y2O3、Ga2O3的元素M2氧化物；
-总计大于1%并低于25%的至少一种选自ZrO2、Ce2O3、HfO2的元素M3氧化物；
-低于20%的SiO2；
所述组成具有:
-低于10%的MgO；
-大于1%并低于20%的Fe2O3；
-大于1%并低于10%的ZrO2；
所述材料通过相应的简单氧化物或者它们的前体之一的反应性烧结或者通过烧结颗粒的热处理获得，所述组成使得a’-t+2m1+m2为-6至6，基于在所述组成中存在的氧化物总量以摩尔%计，其中：
- a是Al2O3的摩尔百分比；
- s是SiO2的摩尔百分比；
- a’=a-0.37×s；
- t是TiO2的摩尔百分比；
- m1是M1的一种或多种氧化物的总摩尔百分比；
- m2是M2的一种或多种氧化物的总摩尔百分比。
2.根据权利要求1的多孔结构，其中M3选自Zr或Zr和Ce的组合，在该材料中ZrO2含量这时大于0.7%。
3. 根据前述权利要求之一的多孔结构，其中M1是Mg，M2包含Fe或是Fe和M3包含Zr或是Zr。
4.根据前述权利要求之一的多孔结构，其中M2由铁和镧的组合构成。
5.根据前述权利要求之一的多孔结构，其中M3由Zr和Ce的组合构成。
6.根据前述权利要求之一的多孔结构，其中所述材料具有以下化学组成，基于氧化物以重量%计：
-大于25%并低于52%的Al2O3；
-大于26%并低于55%的TiO2；
-低于10%的MgO；
-大于1%并低于20%的Fe2O3或(Fe2O3+La2O3)；
-大于1%并低于10%的ZrO2或(ZrO2+CeO2)；
-低于20%的SiO2。
7.根据权利要求6的多孔结构，其中所述材料具有以下化学组成，基于氧化物以重量%计：
-大于35%并低于50%的Al2O3；
-大于26%并低于50%的TiO2；
-低于6%的MgO
-大于2%并低于15%的Fe2O3或(Fe2O3+La2O3)；
-大于2%并低于8%的ZrO2或(ZrO2+CeO2)
-大于0.5%并低于15%的SiO2。
8.根据前述权利要求之一的多孔结构，其包含大于1%的SiO2，优选包含大于3%的SiO2，优选包含大于5%的SiO2。
9.根据前述权利要求之一的多孔结构，其中所述材料包含由含钛、铝、铁、锆和任选的镁的固溶体类型相构成的主相、至少一个基本上由二氧化钛TiO2和/或氧化锆ZrO2组成的相和任选的至少一个含硅酸盐的相。
10.根据权利要求9的多孔结构，其中所述一个或多个含硅酸盐的相的比例可以为该材料总重量的0至45%。
11.根据权利要求10的多孔结构，其中所述含硅酸盐的相主要地由二氧化硅和氧化铝构成，在该含硅酸盐的相中的二氧化硅的重量比例为大于34%。
12.根据前述权利要求之一的多孔结构，其具有蜂窝状类型的结构，特别地用于汽车应用的催化剂载体或过滤器，所述陶瓷材料构成所述具有大于10%的孔隙度和中心在5-60微米的孔径的结构。
Applications Claiming Priority (5)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| FR0956502A FR2950341B1 (fr) | 2009-09-22 | 2009-09-22 | Structure poreuse du type titanate d'alumine |
| FR0956502 | 2009-09-22 | ||
| FR1056155 | 2010-07-27 | ||
| FR1056155 | 2010-07-27 | ||
| PCT/FR2010/051971 WO2011036397A1 (fr) | 2009-09-22 | 2010-09-21 | Structure poreuse du type titanate d'alumine |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102639460A true CN102639460A (zh) | 2012-08-15 |
Family
ID=43382410
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2010800422751A Pending CN102639460A (zh) | 2009-09-22 | 2010-09-21 | 钛酸铝多孔结构 |
Country Status (6)
| Country | Link |
|---|---|
| US (1) | US20120276325A1 (zh) |
| EP (1) | EP2480518A1 (zh) |
| JP (1) | JP5543604B2 (zh) |
| KR (1) | KR20120083349A (zh) |
| CN (1) | CN102639460A (zh) |
| WO (1) | WO2011036397A1 (zh) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106007777A (zh) * | 2016-05-12 | 2016-10-12 | 王维娜 | 一种多孔陶瓷及其制备方法 |
| CN107406328A (zh) * | 2015-03-19 | 2017-11-28 | 衡所华威电子有限公司 | 黑色氧化铝陶瓷粉末、由其制备的黑色氧化铝陶瓷体及制备该黑色氧化铝陶瓷体的方法 |
| CN108946680A (zh) * | 2018-07-03 | 2018-12-07 | 贵州大学 | 一种制备钛酸铝粉体联产酸的工艺 |
| CN111390116A (zh) * | 2020-04-15 | 2020-07-10 | 淄博建宗复合材料有限公司 | 一种钛酸铝陶瓷复合保温冒口的制备工艺流程 |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US9988311B2 (en) * | 2013-11-27 | 2018-06-05 | Corning Incorporated | Aluminum titanate compositions, ceramic articles comprising same, and methods of manufacturing same |
| JP6949019B2 (ja) * | 2016-07-14 | 2021-10-13 | イビデン株式会社 | ハニカム構造体及び該ハニカム構造体の製造方法 |
| JP6692256B2 (ja) * | 2016-08-25 | 2020-05-13 | 日本碍子株式会社 | 多孔質セラミックス構造体 |
| FR3088831B1 (fr) * | 2018-11-27 | 2020-12-04 | Tech Avancees Et Membranes Industrielles | Procédé de fabrication par addition de matière de supports inorganiques de filtration à partir d’un filament thermofusible et membrane obtenue |
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| US6849181B2 (en) | 2002-07-31 | 2005-02-01 | Corning Incorporated | Mullite-aluminum titanate diesel exhaust filter |
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| FR2933400B1 (fr) * | 2008-07-04 | 2010-08-20 | Saint Gobain Ct Recherches | Grains fondus d'oxydes comprenant al, ti, mg et zr et produits ceramiques comportant de tels grains |
| FR2948657B1 (fr) * | 2009-07-28 | 2013-01-04 | Saint Gobain Ct Recherches | Grains fondus d'oxydes comprenant al, ti et produits ceramiques comportant de tels grains |
-
2010
- 2010-09-21 US US13/497,567 patent/US20120276325A1/en not_active Abandoned
- 2010-09-21 EP EP10770601A patent/EP2480518A1/fr not_active Withdrawn
- 2010-09-21 KR KR1020127007311A patent/KR20120083349A/ko not_active Application Discontinuation
- 2010-09-21 WO PCT/FR2010/051971 patent/WO2011036397A1/fr active Application Filing
- 2010-09-21 CN CN2010800422751A patent/CN102639460A/zh active Pending
- 2010-09-21 JP JP2012530316A patent/JP5543604B2/ja not_active Expired - Fee Related
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| US4327188A (en) * | 1979-12-25 | 1982-04-27 | Asahi Glass Company, Ltd. | Multicellular monolithic ceramic body and preparation thereof |
| US4758542A (en) * | 1987-02-13 | 1988-07-19 | W. R. Grace & Co. | Low thermal expansion ZrTiO4 --Al2 TiO5 --ZrO2 compositions |
| CN101357843A (zh) * | 2008-08-08 | 2009-02-04 | 东营新科信特陶有限责任公司 | 钛酸铝陶瓷升液管的制备方法 |
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| CN107406328A (zh) * | 2015-03-19 | 2017-11-28 | 衡所华威电子有限公司 | 黑色氧化铝陶瓷粉末、由其制备的黑色氧化铝陶瓷体及制备该黑色氧化铝陶瓷体的方法 |
| CN106007777A (zh) * | 2016-05-12 | 2016-10-12 | 王维娜 | 一种多孔陶瓷及其制备方法 |
| CN108946680A (zh) * | 2018-07-03 | 2018-12-07 | 贵州大学 | 一种制备钛酸铝粉体联产酸的工艺 |
| CN111390116A (zh) * | 2020-04-15 | 2020-07-10 | 淄博建宗复合材料有限公司 | 一种钛酸铝陶瓷复合保温冒口的制备工艺流程 |
Also Published As
| Publication number | Publication date |
|---|---|
| KR20120083349A (ko) | 2012-07-25 |
| EP2480518A1 (fr) | 2012-08-01 |
| JP5543604B2 (ja) | 2014-07-09 |
| US20120276325A1 (en) | 2012-11-01 |
| WO2011036397A1 (fr) | 2011-03-31 |
| JP2013505197A (ja) | 2013-02-14 |
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