CN102933279B - 陶瓷蜂窝结构体 - Google Patents
陶瓷蜂窝结构体 Download PDFInfo
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- CN102933279B CN102933279B CN201180015699.3A CN201180015699A CN102933279B CN 102933279 B CN102933279 B CN 102933279B CN 201180015699 A CN201180015699 A CN 201180015699A CN 102933279 B CN102933279 B CN 102933279B
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- Prior art keywords
- duct
- ceramic honeycomb
- honeycomb structural
- structural body
- effusion
- Prior art date
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- 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 10
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- INJRKJPEYSAMPD-UHFFFAOYSA-N aluminum;silicic acid;hydrate Chemical compound O.[Al].[Al].O[Si](O)(O)O INJRKJPEYSAMPD-UHFFFAOYSA-N 0.000 claims description 2
- 229910052878 cordierite Inorganic materials 0.000 claims 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 claims description 2
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- ILRRQNADMUWWFW-UHFFFAOYSA-K aluminium phosphate Chemical compound O1[Al]2OP1(=O)O2 ILRRQNADMUWWFW-UHFFFAOYSA-K 0.000 description 1
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- JPNZKPRONVOMLL-UHFFFAOYSA-N azane;octadecanoic acid Chemical compound [NH4+].CCCCCCCCCCCCCCCCCC([O-])=O JPNZKPRONVOMLL-UHFFFAOYSA-N 0.000 description 1
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- WQEPLUUGTLDZJY-UHFFFAOYSA-N n-Pentadecanoic acid Natural products CCCCCCCCCCCCCCC(O)=O WQEPLUUGTLDZJY-UHFFFAOYSA-N 0.000 description 1
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Classifications
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Abstract
本发明提供一种适用于颗粒物过滤器的陶瓷蜂窝结构体,所述陶瓷蜂窝结构体具有进入面和逸出面,包括从所述进入面延伸穿过所述结构体至所述逸出面的多个进入孔道和多个逸出孔道,所述进入孔道在所述进入面处开口并在靠近所述逸出面处封闭,所述逸出孔道在所述逸出面处开口并在靠近所述进入面处封闭。所述进入孔道和所述逸出孔道的截面为四边形,并且以交替样式排布;所述逸出孔道的截面面积通常小于所述进入孔道的截面面积,且具有锐内角,并且任意指定的进入孔道没有一个点距离邻近的进入孔道比距离邻近的逸出孔道更近。本发明还公开了一种用于制备所述陶瓷蜂窝结构体的方法。
Description
技术领域
本发明涉及陶瓷蜂窝结构体,该陶瓷蜂窝结构体包含交替样式的特定形状的进入孔道(inletcell)和逸出孔道(outletcell),本发明还涉及这些结构体的制备方法以及这些结构体在废气颗粒物过滤器(例如柴油机过滤器)中的应用。
背景技术
在本领域中,陶瓷蜂窝结构体常用于制造液态介质和气态介质的过滤器,特别是用于制造从废气中除去细小颗粒的过滤器;这些过滤器位于车辆柴油发动机的排气管道中,用来除去排气中的烟灰成分。这些过滤器可以是整体式或分段式的陶瓷蜂窝体,其包含尺寸通常为500微米~2000微米的孔道或通道,且这些孔道或通道具有受控的壁孔隙率。所述孔道在进入侧和逸出侧交替地进行封堵,从而迫使废气穿过位于通道之间的多孔陶瓷壁,因而在气体穿过所述壁时进行过滤。
适合的蜂窝结构体能提供下述多种所需性质的平衡,所述性质例如:足够的过滤效率,即,经过过滤器的废气应当基本不含柴油机颗粒物;有限的压降,即,过滤器必须显示出使废气流穿过其壁的足够能力;和在较宽的温度范围内对存在于柴油发动机废气中的化合物具有足够的化学耐性。
低热膨胀系数和高耐热冲击性也是所希望的,因为它们能够有助于使过滤器在其寿命期间通常所经历的若干个再生循环后仍然有效,在这些循环中存在快速加热到明显高于正常运行温度的温度的情况。实际上,在过滤行为中,蜂窝结构体的进入通道逐渐被烟灰填满,由此减少了该结构体的过滤行为。因此,必须定期对过滤器进行再生;对过滤器的清洁通过下述方式来进行:将过滤器加热至足以在高温下点燃所收集的柴油机颗粒物的温度(通常高于1000℃),由此使烟灰燃烧。如果过滤器不具有足够的耐热冲击性,机械张力和/或热张力可能引起陶瓷材料的破裂,从而导致过滤效率的下降或丧失,并因此导致过滤器寿命的减少或终止。
为了延长蜂窝过滤器的寿命并提高其过滤效率,本领域中已进行了大量尝试来开发具有改进性质的陶瓷材料,例如碳化硅(SiC)、莫来石、钛酸铝矿(tialite)或硅线石矿物。
进一步的工作已致力于开发不对称的孔道设计,其中,进入孔道大于逸出孔道;本领域中已研究了产生不对称性的两种主要方案。第一种方案包括使用弯曲的通道壁,如在例如EP-A-1676622的图6中所描述的;在这些设计中,通常具有正方形或矩形截面的孔道可以发生部分变形以产生不对称性。图1中还显示,进入孔道的所有侧边都向外鼓起(进入孔道是“膨胀”的),同时逸出孔道的对应侧边则向内鼓起以提供较小的截面面积;结果产生了壁的波状起伏和进入孔道面积略大于逸出孔道的鼓起样式。但是,该设计需要在制造过滤器时使用复杂且昂贵的模具;此外,该结构中积累的诸多限制因素会给陶瓷性能带来问题。该方案的另一个缺点是,相邻的进入通道彼此距离很近,从而降低了过滤效率。因此,已证明这些设计在用于蜂窝过滤器尤其是整体式过滤器时存在缺陷。
本领域中已知的产生不对称性的第二种方案包括使用截面比逸出通道的截面更大的进入通道,如图2所示。例如,WO03/020407描述了一种蜂窝结构体,其孔道通道具有不等的正方形截面。该设计的缺点是,相邻的入口正方形之间的间隔距离变得更小,由此在结构体中形成了可能产生断裂的脆性区域。该缺点可以通过在正方形上产生倒直角并因此形成八边形孔道来得到部分弥补;然而,该倒直角的表面导致过滤效率降低,这是因为与最近的逸出孔道相比,进入孔道壁的很大一部分距离邻近的进入孔道更近,这就需要更长的流动路径来穿过壁。
因此,在本领域中需要具有不对称设计的新型陶瓷蜂窝结构体,其能够提供寿命延长且过滤效率提高的蜂窝过滤器,同时避免了本领域已知的不对称设计中的问题。
发明内容
申请人意外地发现,通过使陶瓷蜂窝结构体具有特定样式的具有特定截面形状的交替状进入孔道和逸出孔道,解决了上述问题。本发明的陶瓷蜂窝结构体具有进入面和逸出面,包括从所述进入面延伸穿过所述结构体至所述逸出面的多个进入孔道和多个逸出孔道,所述进入孔道在所述进入面处开口并在靠近所述逸出面处封闭,所述逸出孔道在所述逸出面处开口并在靠近所述进入面处封闭。
根据第一方面,本发明涉及一种陶瓷蜂窝结构体,其中:
进入孔道和逸出孔道的截面为等边四边形(rhombic),并且以交替样式排布,并且
所述逸出孔道的截面面积通常小于所述进入孔道的截面面积,并且所述逸出孔道具有锐内角。
所述逸出孔道可以具有菱形(diamond)截面,而所述进入孔道可以具有菱形或正方形截面。在本实施方式的陶瓷蜂窝结构体中,优选的是,任意指定的进入孔道没有一个点距离邻近的进入孔道比距离邻近的逸出孔道更近。
根据第二方面,本发明涉及一种陶瓷蜂窝结构体,其中:
进入孔道和逸出孔道以棋盘式布局排布,
所述进入孔道的截面为四边形;并且
沿所述棋盘式布局的指定对角线相邻的进入孔道相对于彼此旋转。
沿所述棋盘式布局的指定对角线相邻的进入孔道以大于1度的角度相对于彼此成角度偏置。
逸出孔道可以具有通常小于进入孔道的截面面积。进入孔道可具有菱形或正方形截面,且优选具有锐内角。在本实施方式的陶瓷蜂窝结构体中,优选的是,任意指定的进入孔道没有一个点距离邻近的进入孔道比距离邻近的逸出孔道更近。
根据第三方面,本发明涉及一种陶瓷蜂窝结构体,其中:
进入孔道和逸出孔道的截面为四边形,并且以交替样式排布,并且
任意指定的进入孔道没有一个点距离邻近的进入孔道比距离邻近的逸出孔道更近。
在本发明的陶瓷蜂窝结构体中,进入孔道和/或逸出孔道可以具有诸如等边四边形或四边形等截面形状,其中一个或多个角是倒直角或圆角。
本发明的蜂窝结构体中孔道的具体几何构造使得逸出/进入比提高、孔道密度升高、过滤表面增大且过滤效率提高;此外,当任意指定的进入孔道没有一个点距离邻近的进入孔道比距离邻近的逸出孔道更近时,蜂窝结构体因热冲击而导致的结构性失效将减少。
本发明还提供一种制造陶瓷蜂窝结构体的方法,所述方法包括以下步骤:
(a)提供蜂窝结构体生坯,所述蜂窝结构体生坯具有本发明上述任一方面所述样式的进入孔道和逸出孔道;
(b)可选地干燥所述蜂窝结构体生坯,并且
(c)烧结所述蜂窝结构体生坯。
在本发明的方法的一个实施方式中,步骤(a)包括提供可挤出的陶瓷混合物并挤出所述混合物以形成所述蜂窝结构体生坯。
本发明还提供一种柴油机颗粒物过滤器,其包含一个或多个本发明上述任一方面所述的陶瓷蜂窝结构体。
附图说明
图1和图2示出了不是本发明的进入通道和逸出通道的不对称设计的放大示意平面图。
图3~图6是本发明的陶瓷蜂窝结构体中进入孔道和逸出孔道的不对称设计的放大示意平面图。
具体实施方式
根据第一方面,本发明涉及一种陶瓷蜂窝结构体,其中,进入孔道和逸出孔道的截面均为等边四边形,并且以交替样式排布,其中所述逸出孔道的截面面积通常小于所述进入孔道的截面面积,并且具有锐内角。
逸出孔道的菱形截面优选具有锐内角(α);进入孔道可以具有菱形或正方形截面,且优选具有锐内角(β)。在本实施方式的陶瓷蜂窝结构体中,优选的是,任意指定的进入孔道没有一个点距离邻近的进入孔道比距离邻近的逸出孔道更近。
根据本发明的第二方面,进入孔道和逸出孔道以棋盘式布局排布;进入孔道的截面为四边形,并且沿棋盘式布局的指定对角线相邻的进入孔道以大于1度的角度相对于彼此旋转。沿棋盘式布局的指定对角线相邻的进入孔道以大于1度的角度成角度偏置;所述“角度偏置”(angularoffset)是指相邻的进入孔道的对角线的垂线发生偏向。进入孔道可具有正方形或菱形的截面,且优选具有锐内角(β)。当进入孔道具有菱形截面时,所述“角度偏置”是指相邻的进入孔道的两条主对角线的垂线发生偏向。孔道的主对角线是指该孔道的两条对角线中较长的一条对角线。优选的是,沿棋盘式布局的指定对角线相邻的进入孔道的主对角线以1度~30度,或3度~20度成角度偏置。
逸出孔道的截面面积通常可以小于进入孔道的截面面积。逸出孔道可以是正方形、矩形、八边形、多边形或适合于以重复性样式进行排布的其他任何形状或形状组合;逸出孔道的截面优选为四边形。逸出孔道可以具有锐内角(α),优选小于(β);沿棋盘式布局的指定对角线相邻的进入孔道可以以等于90-(α)的角度成角度偏置。在本实施方式的陶瓷蜂窝结构体中,优选的是,任意指定的进入孔道没有一个点距离邻近的进入孔道比距离邻近的逸出孔道更近。
根据本发明的第三方面,进入孔道和逸出孔道的截面为四边形,并且以交替样式排布,并且任意指定的进入孔道没有一个点距离邻近的进入孔道比距离邻近的逸出孔道更近。
在上述的本发明任一方面的陶瓷蜂窝结构体中,进入孔道和/或逸出孔道的截面形状可以具有一个或多个倒直角或圆角。
用于获得上述的本发明任一方面的构造的孔道截面形状没有特别限制;孔道截面形状的实例包括等边四边形和矩形。“等边四边形”意思是所有边长都相等的四边形,例如正方形或菱形。
进入孔道和逸出孔道优选具有菱形截面,其中逸出孔道具有锐角(α),进入孔道具有锐角(β),逸出孔道和进入孔道被直壁分隔开。这些菱形优选排列成以下形式:四个(α)菱形在其之间界定一个(β)菱形,反之亦然。(β)优选大于(α)。逸出孔道的锐内角(α)可以是50度~85度、优选为60度~85度。
在本发明的上述任一方面的陶瓷蜂窝结构体中,过滤器每单位体积的过滤面积(surface)(以mm2/mm3表示)可以是0.8~1。
开口率(apertureratio)的定义为进入通道的截面面积与过滤器的总截面面积之比,其可以大于35%;开口率优选小于45%。该比值通常通过以下方法测得:用过滤器的一个单元孔道(该单元孔道按照表示过滤器总表面的需要而多次重现)中的进入通道的面积除以该单元孔道的面积,再乘以100。
根据DIN51045用膨胀法测得的本发明的上述任一方面的陶瓷蜂窝结构体的热膨胀系数可以是0~9×10-6K-1,或4.5×10-6K-1~7×10-6K-1。
图3和图4显示了本发明的进入孔道和逸出孔道的排布方式的变型,但还可以使用多种其他构造。对孔道样式的描述是假设在垂直于蜂窝结构体纵向轴的延伸平面中观察这些孔道的情况下而给出的。进入孔道中有阴影,以表示它们在其出口末端是阻塞的;而逸出通道中空白,表示它们在其出口末端是开放的。蜂窝结构体可以是具有圆形外周壁的圆柱体;外周壁可以采用任何所需的曲形或几何外形,例如椭圆形、卵形、矩形或三角形等。
图3显示了进入孔道和逸出孔道的形状为等边四边形的蜂窝结构体的部分截面示意图。进入孔道的锐内角(β)为84度,而逸出孔道的锐内角(α)为69度;因此,(β)大于(α)。
在图4的实施方式中,进入孔道和逸出孔道的截面具有圆角等边四边形,并在截面图中以棋盘式样式排布。进入孔道的锐内角(β)为83度,而逸出孔道的锐内角(α)为70度;因此,(β)大于(α)。进入孔道和逸出孔道以横排和竖排排布,且进入孔道按照棋盘式样式与逸出孔道交错。蜂窝结构体的各个内部壁部分在其表面的所有点处(除了如在孔道的拐角处那样与其他壁连接的部位)都位于进入孔道和逸出孔道之间;因此,除了拐角连接,进入孔道通过***逸出孔道之间而彼此间隔,反之亦然。沿棋盘式布局的指定对角线上设置的相邻进入孔道的主对角线以20度(即90-(α))的角度成角度偏置。如上所述,“角度偏置”是指相邻的进入孔道的对角线的垂线发生偏向。
本发明的陶瓷蜂窝结构体的新型孔道构造提供了更大的自由度和更大的可能性使过滤器适应于过滤用途的要求,特别是孔道壁厚、逸出孔道的锐内角(α)、进入孔道的锐内角(β)和相邻的进入孔道的间距的要求。这种新型孔道构造还提供了以下优点:对于一定的孔道入口截面面积,提高了孔道密度(以每平方厘米的孔道数量计,或以每平方英寸的孔道数量(cpsi)计),并提高了孔径比。特别地,(α)角和(β)角越小,对于一定的菱形侧边长度而言孔道密度就越大。(β)/(α)比值越大,蜂窝结构体的逸出/进入比就越大。
此外,本发明的方案避免了对倒直角的使用,因此避免了过滤面积的任何损失。整个壁表面都可用于过滤,因为任意指定的进入通道没有一个点距离邻近的进入孔道比距离邻近的逸出孔道更近。气流以梯形形状从进入通道传送至逸出通道。
此外,本发明的陶瓷蜂窝结构体可以具有非常均一的壁厚。可以容易地将孔道构造的参数调整为使壁厚在整个设计中保持恒定。这样能够获得不具有特定的壁累积点(厚度增加)的结构体,该壁累积点可以造成废气流的不连续性和由此导致的烟灰积累,而且可以在再生阶段产生特定的热点。
在本发明的蜂窝结构体中,纵向上并排的进入孔道和逸出孔道可以由多孔壁分隔开,并且可以以上述交替的方式将其封堵。蜂窝结构体的内部壁可以是多孔的,从而允许废气从进入孔道穿过这些壁到达逸出孔道。适当地确定壁的孔隙率大小以滤出废气中存在的大部分颗粒物。
本发明的陶瓷蜂窝结构体的总孔隙率可以是20%~80%,或35%~70%,总孔隙率用汞孔率测定法测得(体积百分比基于矿物相和孔隙的总体积计算出)。孔隙率由使用ThermoScientific的汞孔率计Pascal140以130度的接触角测得的汞扩散率来确定。用汞孔率测定法测得的孔直径d50可以是1微米~60微米,或5微米~50微米,或8微米~30微米。根据陶瓷蜂窝体的设计用途,特别是针对是否将陶瓷蜂窝结构体进一步浸入例如催化剂的问题,上述数值可以有所变化。对于非浸渍型陶瓷蜂窝结构体,孔直径通常为10微米~20微米;对于浸渍型结构体,浸渍前的孔直径通常为20微米~25微米。沉积在孔隙内的催化剂物质将使原始孔直径变小。
本发明的蜂窝过滤器的平均孔道密度没有限制。陶瓷蜂窝结构体的孔道密度可以是6孔道/平方英寸~2000孔道/平方英寸(0.9孔道/cm2~311孔道/cm2),或50孔道/平方英寸~1000孔道/平方英寸(7.8孔道/cm2~155孔道/cm2),或100孔道/平方英寸~400孔道/平方英寸(15.5孔道/cm2~62.0孔道/cm2)。孔道密度的定义为:烧结后的过滤器的入口或出口的面积除以两个进入通道和两个逸出通道以及连接壁的面积,所得到的比值再乘以4。所述连接壁是与孔道邻接的壁,其选择方式使得由进入孔道和逸出孔道以及连接壁构成的单元图样能够按转变成棋盘式布局的需要多次重现。
将本发明的相邻孔道分隔开的间隔壁的厚度没有限制。间隔壁的厚度可以是100微米~500微米,或200微米~450微米。
此外,结构体的外周壁优选比间隔壁厚,其厚度可以是100微米~700微米,或200微米~400微米。所述外周壁不仅可以是在成型时与间隔壁一体成型的壁,而且可以是通过将外周打磨成预定形状而成型的涂覆结合剂的壁。
孔道的表面粗糙度Ra可以是1微米~100微米,或10微米~50微米,该表面粗糙度Ra依照JISB0601(1994)测得。
在本发明中,构成蜂窝结构体的材料没有限制;本发明的蜂窝结构体可以由任何适合的陶瓷材料构成。适合的陶瓷材料包括碳化硅(SiC)、氮化硅、莫来石、堇青石、氧化锆、二氧化钛、二氧化硅、氧化镁、氧化铝、尖晶石、钛酸铝矿、蓝晶石、硅线石、红柱石、锂铝硅酸盐、铝钛酸盐及其混合物。陶瓷材料可以含有金属,例如Fe-Cr-Al基金属和金属硅等。
根据优选实施方式,陶瓷材料包含大量的莫来石相和少量的钛酸铝矿(即,莫来石相为主导相),如WO2009/076985(通过援引将其内容并入本文)中所述;该陶瓷材料提供了增大的机械强度和高耐热冲击性。
陶瓷蜂窝结构体可以包含莫来石的矿物相和钛酸铝矿的矿物相,其中莫来石与钛酸铝矿的体积比≥2:1,或≥4:1,或≥10:1。钛酸铝矿相可以被莫来石相包围,并且可以是基本平行的晶体形式。陶瓷蜂窝结构体中的莫来石的量可以大于50体积%,或大于75体积%,或甚至大于80体积%(基于蜂窝体的矿物相的总体积计算)。
陶瓷蜂窝结构体可以包含由红柱石组成的矿物相;红柱石相的存在量可以是0.5体积%~低于50体积%,或者是5体积%~30体积%,或0.5体积%~15体积%(基于陶瓷蜂窝结构体的固相体积)。适合的含红柱石的陶瓷蜂窝结构体包含:
-0.5%~15.0%或5.0%~8.0%的红柱石;
-60.0%~90.0%或75.0%~90.0%的莫来石;
-2.5%~20.0%或4.0%~7.0%的钛酸铝矿;
-0~2.0%的金红石和/或锐钛矿;和
-3.0%~20.0%的非晶二氧化硅相;
其中,上述成分的总量为100体积%(基于固体化合物的体积)。
通过密封孔道而形成的密封部的材料没有限制,但该材料优选包含选自优选用于蜂窝结构体的间隔壁的上述陶瓷和金属中的一种或多种陶瓷和/或金属。
本发明用于制造上述陶瓷蜂窝结构体的方法包括以下步骤:
(a)提供具有上述呈交替样式的进入孔道和逸出孔道的蜂窝结构体生坯;
(b)可选地干燥所述蜂窝结构体生坯,并且
(c)烧结所述蜂窝结构体生坯。
步骤(a)可以包括提供可挤出的陶瓷混合物并挤出所述混合物以形成所述蜂窝结构体生坯。
所述可挤出的混合物或所述蜂窝结构体生坯可以包含一种或多种粘合剂;粘合剂的作用是在加热或烧结步骤前的过程步骤中为蜂窝结构体生坯提供足够的机械稳定性。适合的粘合剂可以选自由甲基纤维素、羟甲基丙基纤维素、聚乙烯醇缩丁醛、乳化丙烯酸酯、聚乙烯醇、聚乙烯吡咯烷酮、聚丙烯酸化物、淀粉、硅粘合剂、聚丙烯酸酯、硅酸盐、聚乙烯亚胺、木质素磺酸盐、藻酸盐及其混合物组成的组。粘合剂的总存在量可以是1.5重量%~15重量%,或2重量%~9重量%(基于可挤出的混合物或蜂窝结构体生坯的干重)。
可挤出的混合物或蜂窝结构体生坯可以包含一种或多种无机粘合剂;适合的无机粘合剂可以选自包括但不限于膨润土、磷酸铝、伯姆石、硅酸钠、硅酸硼及其混合物的组。
可挤出的混合物或蜂窝结构体生坯可以包含一种或多种辅助剂,所述辅助剂在挤出步骤中为原料提供有利的性质(增塑剂、助流剂和润滑剂等)。适合的辅助剂可以选自由聚乙二醇(PEG)、甘油、乙二醇、邻苯二甲酸辛酯、硬脂酸铵、蜡乳化液、油酸、Manhattan鱼油、硬脂酸、蜡、棕榈酸、亚油酸、肉豆蔻酸、月桂酸及其混合物组成的组。辅助剂的存在总量可以是1.5重量%~15重量%,或2重量%~9重量%(基于可挤出的混合物或蜂窝结构体生坯的干重;如果使用液体辅助剂,其重量也纳入在可挤出的混合物或蜂窝结构体生坯的干重中)。可挤出的混合物或蜂窝结构体生坯的“干重”是指适合用于可挤出的混合物中的本文所讨论的任何化合物的总重量,即,矿物相和粘合剂/辅助剂的总重量。因此,“干重”应理解为包括在环境条件下呈液态的辅助剂,但不包括矿物、粘合剂或辅助剂的水溶液中的水(如果使用这些水溶液来制备所述混合物)。
根据本领域已知的方法和技术,由矿物化合物(可选地与粘合剂和/或辅助剂一起)制备可挤出的混合物。可以在常规捏合机中按需添加足量的合适的液相(通常为水)来混合原料,从而得到适于挤出的浆料。此外,可以使用本领域中已知的常规挤出设备(例如螺旋挤出机)和用于挤出蜂窝结构体的模具。上述技术的综述参见教材W.Kollenberg(编),TechnischeKeramik,Vulkan-Verlag,Essen,Germany,2004,并通过援引将其并入本文。
蜂窝结构体生坯的直径和配置可以通过选择具有所需尺寸和形状的挤出机模具来确定。可以使用具有以四边形对称形式排布的顶针(pin)的挤出模具来制造蜂窝结构体。所述顶针的角可以是圆角或不是圆角。
在挤出后,所挤出的物质被切割成具有适合长度的片段以获得具有所需式样的蜂窝结构体生坯。该步骤中的适合的切割工具(例如剪钳)是本领域技术人员已知的。
在本发明的方法的可选步骤(b)中,在烧结前,可以根据本领域中已知的方法(例如微波干燥、热空气干燥)来干燥所挤出的蜂窝结构体生坯。作为另一选择,干燥步骤可以按下述方式进行:在人工气候室中,使蜂窝结构体生坯在20℃~90℃的预定温度下长时间地暴露于具有受控湿度的气氛中,其中,逐步降低周围空气的湿度,同时相应地升高温度。例如,本发明的蜂窝结构体生坯的一种干燥程序如下:
-在室温下保持70%的相对空气湿度48小时;
-在50℃下保持60%的相对空气湿度3小时;
-在75℃下保持50%的相对空气湿度3小时;并且
-在85℃下保持50%的相对空气湿度12小时。
随后,可以在用于制备陶瓷材料的常规烘箱或烧窑中加热经干燥的蜂窝结构体生坯。通常,适于使受热物体处于预定温度的任何烘箱或烧窑都适合于本发明的方法。
当蜂窝结构体生坯包含有机粘合剂化合物和/或有机辅助剂时,通常在将该结构体加热至最终的烧结温度前,先将该结构体加热至200℃~300℃的温度,并且将该温度保持一段时间,这段时间足以通过燃烧除去有机粘合剂和辅助剂化合物(例如1~3小时)。
烧结步骤(c)可以在1250℃~1700℃、或1350℃~1600℃、或1400℃~1580℃、或1400℃~1500℃的温度下进行。根据一个实施方式,上述方法在烧结步骤前包括将蜂窝结构体生坯加热至650℃~950℃、或700℃~900℃、或800℃~850℃的温度的步骤。
对于作为柴油机颗粒物过滤器的应用而言,可以对本发明的陶瓷蜂窝结构体或陶瓷蜂窝结构体生坯进一步进行封堵处理,即用额外的陶瓷材料(mass)在预定的位置封闭蜂窝体的某些开口结构。因此,封堵过程包括:制备适合的封堵材料,将所述封堵材料施加至陶瓷蜂窝结构体或蜂窝结构体生坯的所需位置,并对封堵后的蜂窝结构体进行额外的烧结步骤,或在一个步骤中对封堵后的蜂窝结构体生坯进行烧结,其中,将所述封堵材料将转化为具有适用于柴油机颗粒物过滤器的性质的陶瓷封堵材料。并不要求陶瓷封堵材料的成分与蜂窝体的陶瓷材料成分相同。通常,可以使用本领域技术人员已知的封堵方法和封堵材料来封堵本发明的蜂窝体。
随后,可以将封堵后的陶瓷蜂窝结构体固定在适合于将所述结构体安装到柴油发动机废气管道中的箱壳中。
本发明的另一个目的是包含一个或多个上述陶瓷蜂窝结构体的颗粒物过滤器;该过滤器可以是例如柴油机颗粒物过滤器或用于从废气中除去NOx的选择性催化还原型过滤器。
颗粒物过滤器可以由本发明的一个陶瓷蜂窝结构体以整体形式成型,或者可以由多个一体化的结构体组成。在后一种情况下,如果将蜂窝过滤器分段并随后一体化,对各结构体的尺寸和形状没有限制;各结构体的截面面积可以是900mm2~10000mm2,或900mm2~5000mm2,或900mm2~3600mm2。作为结构体的优选形状,例如,截面形状为四边形。颗粒物过滤器的整体截面形状没有特别限制,其形状可以是圆形、椭圆形、四边形和多边形。为了使颗粒物过滤器成型为多个结构体一体化的构造,在获得上述结构体后,可以使用例如陶瓷结合剂粘接这些结构体,并对其进行干燥/硬化,从而获得过滤器。
实施例
以下实施例并不试图限制本发明的范围,其示出了本发明的蜂窝结构体的孔道几何构造相对于现有技术所获得的优势。
实施例1
对具有符合表1所列参数的构造的本发明的蜂窝结构体进行了评估;参数α、β、a、e、f的含义如图5所示。进入孔道菱形的边长可计算为(a-2f),逸出孔道菱形的边长可计算为(a-2e)。
表1
在下表2中,本发明的蜂窝构造与现有技术的正方形设计(其中(α)和(β)为90度)进行了比较。
表2
在表2中,前三行的蜂窝构造以恒定的壁截面面积制造,而后三行的蜂窝构造以恒定的壁厚制造。如上表所示,本发明(α)为65度且(β)为90度或80度的蜂窝构造提供了比现有技术的正方形设计大得多的过滤面积。此外,如表2所示,本发明的蜂窝构造提供了改善的不对称比和更高的孔道密度,由此提供了增大的过滤面积。
以上实例表明本发明的蜂窝构造能够实现合适的不对称比,其中逸出孔道水力直径约为1000微米且过滤面积甚至大于0.98。以上实例还显示出本发明的蜂窝结构体构造所提供的自由度;具体而言,一旦确定了壁所占据的空间,则可以通过改变(α)角和(β)角容易地调整进入孔道面积和逸出孔道面积。与现有技术中的倒直角设计相比,本发明的蜂窝结构体构造能够获得增大的过滤面积和提高的过滤效率,这是因为不存在因倒直角造成的过滤效率损失。
最后,在以下不等式(1)和不等式(2)成立时,获得了本发明的蜂窝构造,其中,任意指定的进入孔道没有一个点距离邻近的进入孔道比距离邻近的逸出孔道更近:
(1)f>e(1-cosα)/(1+cosβ)和
(2)f>e(1+cosα)/(1-cosβ)。
实施例2
对进入孔道和逸出孔道具有圆角的本发明的蜂窝结构体进行评估;蜂窝构造和参数α、β、a、e和f参见表3和图6。这些蜂窝结构体提供了制造优势,因为具有可变直径的电极(electrode)A和B可以用于制备不对称孔道;在本发明的实施方式中,电极A和B的半径均为100微米。
表3
在上述构造中,使壁所占据的总空间保持恒定,与具有尖角的对应结构体相比,上述构造提供了更大的进入通道。其中(α)为65度且(β)为70度、75度或80度的构造提供了高过滤面积、高孔道密度和改善的逸出/进入比的最佳平衡。
出于说明目的,上文的描述涉及了本发明的特定实施方式。然而,显而易见的是,对于本领域技术人员而言,可以对本文所描述的实施方式进行多种修改和变形。所有这些修改和变形均应包含在所附权利要求所界定的本发明的范围内。
Claims (18)
1.一种陶瓷蜂窝结构体,所述陶瓷蜂窝结构体具有进入面和逸出面,包括从所述进入面延伸穿过所述结构体至所述逸出面的多个进入孔道和多个逸出孔道,所述进入孔道在所述进入面处开口并在靠近所述逸出面处封闭,所述逸出孔道在所述逸出面处开口并在靠近所述进入面处封闭,其中:
所述进入孔道和所述逸出孔道以棋盘式布局的方式排布,
所述进入孔道的截面为四边形;并且
沿所述棋盘式布局的指定对角线相邻的进入孔道相对于彼此旋转。
2.如权利要求1所述的陶瓷蜂窝结构体,其中,沿所述棋盘式布局的指定对角线相邻的进入孔道以大于1度的角度相对于彼此旋转。
3.如权利要求1或2所述的陶瓷蜂窝结构体,其中,任意指定的进入孔道没有一个点距离邻近的进入孔道比距离邻近的逸出孔道更近。
4.如权利要求1或2所述的陶瓷蜂窝结构体,其中,过滤器每单位体积的过滤面积是0.8mm2/mm3~1mm2/mm3。
5.如权利要求1或2所述的陶瓷蜂窝结构体,其中,开口率大于35%。
6.如权利要求1或2所述的陶瓷蜂窝结构体,其中,所述逸出孔道的锐内角(α)为50度~85度。
7.如权利要求1或2所述的陶瓷蜂窝结构体,其中,所述进入孔道具有锐内角(β)且所述逸出孔道具有锐内角(α),并且(β)大于(α)。
8.如权利要求1或2所述的陶瓷蜂窝结构体,其中,四边形的进入孔道具有一个或多个倒直角或圆角。
9.如权利要求8所述的陶瓷蜂窝结构体,其中,所述四边形为等边四边形。
10.如权利要求1或2所述的陶瓷蜂窝结构体,其中,相邻的孔道由厚度为100微米~500微米的间隔壁分隔开。
11.如权利要求1或2所述的陶瓷蜂窝结构体,所述陶瓷蜂窝结构体包含一种或多种矿物,所述矿物选自由碳化硅(SiC)、氮化硅、莫来石、堇青石、氧化锆、二氧化钛、二氧化硅、氧化镁、氧化铝、尖晶石、钛酸铝矿、蓝晶石、硅线石、红柱石、锂铝硅酸盐和铝钛酸盐组成的组。
12.如权利要求1或2所述的陶瓷蜂窝结构体,所述陶瓷蜂窝结构体的热膨胀系数为0~9×10-6K-1。
13.如权利要求1或2所述的陶瓷蜂窝结构体,其中,进入孔道和逸出孔道的表面粗糙度Ra为1微米~100微米。
14.如权利要求1或2所述的陶瓷蜂窝结构体,所述陶瓷蜂窝结构体的总孔隙率为20%~80%。
15.如权利要求1或2所述的陶瓷蜂窝结构体,所述陶瓷蜂窝结构体的孔直径d50为1微米~60微米。
16.一种制造前述权利要求中任一项所述的陶瓷蜂窝结构体的方法,所述方法包括以下步骤:
(a)提供蜂窝结构体生坯,所述蜂窝结构体生坯具有权利要求1~10中任一项所限定样式的进入孔道和逸出孔道;
(b)可选地干燥所述蜂窝结构体生坯,并且
(c)烧结所述蜂窝结构体生坯。
17.如权利要求16所述的方法,其中,所述步骤(a)包括提供可挤出的陶瓷混合物并挤出所述混合物以形成所述蜂窝结构体生坯。
18.一种颗粒物过滤器,所述颗粒物过滤器包含一个或多个陶瓷蜂窝结构体,所述陶瓷蜂窝结构体为权利要求1~15中任一项所述的陶瓷蜂窝结构体。
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PCT/EP2011/054619 WO2011117385A1 (en) | 2010-03-26 | 2011-03-25 | Ceramic honeycomb structures |
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WO2011117385A1 (en) | 2011-09-29 |
US8888883B2 (en) | 2014-11-18 |
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