CN103702960A - 生产胶结并具有表皮的陶瓷蜂窝结构的方法 - Google Patents
生产胶结并具有表皮的陶瓷蜂窝结构的方法 Download PDFInfo
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- CN103702960A CN103702960A CN201280036125.9A CN201280036125A CN103702960A CN 103702960 A CN103702960 A CN 103702960A CN 201280036125 A CN201280036125 A CN 201280036125A CN 103702960 A CN103702960 A CN 103702960A
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- honeycomb
- jointing compound
- organic polymer
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- ceramic honeycomb
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Abstract
在用于向陶瓷蜂窝施加表皮、或将所述陶瓷蜂窝与另外的蜂窝或另一种材料粘合的胶结剂组合物中提供有机聚合物粒子。所述有机聚合物粒子的存在减少了所述胶结剂组合物渗透过所述蜂窝的多孔壁。以这种方式,看到蜂窝巢室堵塞较少,并且减少了当胶结剂组合物施加于陶瓷蜂窝时经常看到的热冲击性能降低。
Description
本申请要求2011年7月22日提交的美国临时申请No.61/510,811的优先权。
本发明涉及制造陶瓷蜂窝结构的方法。
具有薄壁、开放巢室(cell)的蜂窝状结构广泛地用作过滤器和作为催化剂载体应用。它们经常通过过滤掉微粒(例如烟尘粒子)和/或气溶胶微滴用于处理燃烧气体,或作为将排气的某些组分(例如NOx化合物)催化转化成无害化合物(例如N2和H2O)的催化材料的载体。这些蜂窝状结构经常被称为“壁流”装置,因为所述巢室壁是多孔的并且当应用所述结构时气体透过所述壁。流体在它们透过所述多孔壁时被过滤和/或接触活性催化剂材料。
用于处理燃烧气体的蜂窝通常由陶瓷材料制成,因为所述蜂窝在它使用期间要经历高温。
陶瓷蜂窝以挤塑方法制造。前体材料、液体(通常是水)、通常致孔剂和一种或多种粘合剂的可挤塑混合物通过模头挤出,形成具有所需的蜂窝结构的生坯。生坯然后在一个或多个步骤中焙烧,形成陶瓷蜂窝。
胶结剂经常施加于所述蜂窝,主要是出于两种原因。首先,陶瓷“表皮”通常施加于蜂窝结构周缘。这防止气体从蜂窝的侧面逸出。所述“表皮”通过焙烧包含无机粘合剂和通常一些陶瓷纤维的胶结材料而制成。其次,在有些情况下,两个或更多个较小的蜂窝被胶结在一起形成较大的蜂窝结构。这允许由较容易生产的较小节段构造较大的蜂窝。这样做的另一个优点是以这种方式制造的分段式蜂窝比整块式蜂窝更抗热冲击。所述胶结剂组合物,如“表皮”组合物,包含无机粘合剂,并且被焙烧以产生所述胶结剂。
在所述表皮或胶结剂施加过程期间,所述粘合剂由于毛细作用迁移通过蜂窝结构的孔隙,并渗入相邻的巢室中。当焙烧所述胶结组合物时,以这种方式迁移的粘合剂部分或完全地堵塞那些巢室。这引起了若干问题。穿过所述堵塞或部分堵塞的巢室、以及作为整体的蜂窝结构有较高的压降。因此,需要更多的功迫使气体通过所述过滤器。在内燃机环境下,这导致燃料效率损失。
堵塞或部分堵塞的巢室还可以以几种方式降低所述过滤器的热稳固性。所述堵塞减少了气流通过受影响的巢室,这可产生局部较高或较低的温度以及整个所述过滤器中更高的温度梯度。由于所述堵塞的或部分堵塞的巢室,捕获的烟尘或其它粒子在整个过滤器中变得分布不均匀。另外,由于存在从胶结剂迁移进入的无机粘合剂,蜂窝基材的弹性模量局部变得较高。这可导致在所述过滤器局部部分的材料热冲击性能降低。所有这些因素可促进机械和/或热故障。
因为较难以在堵塞的或部分堵塞的巢室中产生必要的再生温度,所以所述堵塞的或部分堵塞的巢室也降低了再生效率。
因此,希望找到一种经济有效的方式来减少那些粘合剂迁移到蜂窝结构的巢室中。
实现它的一种方式是引入阻断粘合剂通过蜂窝壁的孔隙的物理屏障。在这种方式中,聚合涂层被施加于待施加胶结剂的蜂窝结构表面。胶结剂则施加在所述聚合涂层上,并且所述涂层在焙烧所述胶结剂时或之前被烧掉。这种方式是有效的,但是需要进行几个附加的加工步骤(施加并干燥所述聚合物涂层),因此增加了生产成本。需要的是更便宜然而有效的防止粘合剂迁移的方式。
本发明是将胶结层施加到多孔陶瓷蜂窝结构上的方法,所述方法包括以下步骤:(a)向陶瓷蜂窝的至少一个多孔表面施加胶结剂组合物,所述陶瓷蜂窝包含由相交的多孔壁限定的多个轴向延伸的巢室,和(b)焙烧所述蜂窝和胶结剂组合物,其中所述胶结剂组合物含有至少一种无机粘合剂、至少一种无机填充剂、载液和分散在所述载液中的粒度从约10纳米至100微米的有机聚合物粒子。
已经发现,在所述胶结剂组合物中存在少量有机聚合物粒子非常有效地减少了无机粘合剂迁移通过蜂窝壁的孔隙。于是,较少的巢室发生堵塞,并且改善了与堵塞有关的问题。这种结果相当令人惊讶,因为,与以前的方法不同,在施加胶结剂组合物之前没有向所述蜂窝施加聚合物层并且干燥。相反,在胶结剂组合物中存在所述聚合物粒子足以减少粘合剂迁移。粘合剂迁移减少导致较少的巢室堵塞,这进而导致通过所述过滤器的较小的压降,并在蜂窝使用和/或再生时在所述蜂窝内产生较小的温度梯度。因为粘合剂迁移减少,底下的蜂窝基材的弹性模量很少或没有出现增加,并且没有显著危害蜂窝的抗热冲击性。
所述陶瓷蜂窝的特征在于具有轴向延伸通过蜂窝体长度的多个巢室。所述巢室由多个同样轴向延伸通过所述蜂窝长度的相交壁限定。所述壁和所述交点限定巢室的数量以及它们的横截面形状和尺寸。许多过滤或催化应用中的典型的蜂窝将含有25至1000个巢室/平方英寸(约4至150个巢室/平方厘米)横截面积(即横截所述巢室的纵向延伸)。壁厚通常为0.05至10mm,优选从0.2至1mm,虽然更大或更小的壁厚也可能使用。
所述陶瓷蜂窝的壁是多孔的。壁的孔隙度可以低到5体积%或高达约90体积%。优选的孔隙度是至少25体积%,更优选的孔隙度是至少40体积%和还更优选的孔隙度是至少50体积%。孔隙度可通过各种浸没法或水银孔率法测量。所述壁孔隙的体积平均孔径是至少5微米并尤其是至少10微米,最多50微米,最多35微米或最多25微米。“孔径”为了本发明的目的表示为通过水银孔率法(其假定圆柱形孔隙)测量的表观体积平均孔径。
所述陶瓷蜂窝可以是整块的(即在单片中形成),或可以是较小蜂窝的组件,所述较小蜂窝单独制造然后通常利用陶瓷胶结剂组装在一起。在这样的组件中的陶瓷胶结剂在一些实施方式中是如本文中所述的焙烧胶结剂组合物。
所述陶瓷蜂窝可以由无机材料例如氧化铝、氧化锆、碳化硅、氮化硅、氮化铝、氮氧化硅、碳氮化硅、莫来石、堇青石、β-锂辉石、钛酸铝、硅酸锶铝或硅酸锂铝制成。在优选实施方式中,所述陶瓷蜂窝的至少一部分是针状莫来石。在一些实施方式中,针状莫来石蜂窝将含有至少0.5重量%残余氟,它是在氟黄玉(fluorotopaz)分解形成针状莫来石针结构之后残留的。
所述胶结剂组合物含有至少一种无机粘合剂、至少一种无机填充剂、载液和分散在所述载液中的粒度为约10纳米至100微米的有机聚合物粒子。
合适的无机粘合剂是在焙烧所述胶结剂组合物时形成玻璃状粘合剂相的材料。合适的粘合剂包括胶态二氧化硅、胶态氧化铝、或胶态二氧化硅和胶态氧化铝的混合物。
无机粘合剂可以占所述胶结剂组合物的固体部分重量的10至70%,优选15至50%并更优选20至40%。所述组合物中的“固体”是在焙烧步骤完成之后残留的那些无机材料。
所述无机填充剂粒子是在焙烧胶结剂组合物时不形成粘合相的材料,并因此区别于所述胶结剂组合物的无机粘合剂组分。所述无机填充剂粒子在整个焙烧过程中反而保持它们的微粒本质,虽然它们可以通过所述粘合相与其它粒子或与无机纤维结合。
所述填充剂粒子可以是非晶的、部分结晶或完全结晶的。所述无机填充剂粒子可以含有被玻璃包围的结晶相。所述填充剂粒子可以具有与陶瓷蜂窝的热膨胀系数非常匹配的热膨胀系数。在200℃至600℃的温度范围内,所述填充剂粒子的平均热膨胀系数可以,例如,与陶瓷蜂窝相差不超过2ppm/℃,优选不超过1ppm/℃。在一些实施方式中,所述填充剂粒子可以是与陶瓷蜂窝相同的材料。
合适的无机填充剂粒子包括铝酸盐、硅酸盐或铝硅酸盐材料,它们也可以含有其它元素例如稀土、锆、铁、硼和碱土。可用作无机填充剂粒子的铝酸盐、硅酸盐或铝硅酸盐材料的例子是氧化铝、硼硅玻璃、石英、e-玻璃、s-玻璃、碳化硅、氮化硅、莫来石、堇青石、硅酸铝、氧化铝-氧化锆-硅酸盐、硅酸锶铝、硅酸锂铝、硅灰石、玄武岩和钛酸铝。
其它合适的无机填充剂粒子包括氧化锆、碳化硅、碳化钛、碳化铝、碳化硼、氮化硅、氮化铝、氮化硼、氮氧化硅、碳氮化硅、堇青石、β-锂辉石等等。
所述无机填充剂粒子可以至少部分是纤维的形式,所述纤维直径为从100纳米至20微米并且纵横比(最长维度除以最短维度)为至少10、优选至少20。优选的纤维直径是0.5至10微米。更优选的纤维直径是3至10微米。这样的无机纤维的数均长度可以为100微米至130毫米或更长。在本发明的一些实施方式中,基本所有的所述纤维的长度都小于1mm。在其它实施方式中,所述纤维具有双峰或多峰长度分布,其中一部分纤维是数均长度为100至1000微米的较短纤维,并且至少其它一部分纤维是较长纤维,其数均长度为至少1毫米、优选1至100毫米、更优选2至100毫米并且甚至更优选5至30毫米。在这样的实施方式中,较长纤维优选占无机纤维总重量的1至50、更优选3至30并且甚至更优选5至25%。
有用的无机纤维的例子包括莫来石纤维,例如可得自Unifrax;氧化铝-锆-硅酸盐纤维,例如可得自Unifrax;含有最多10重量%二氧化硅的氧化铝纤维,例如可得自Saffil;γ-氧化铝和α-氧化铝+莫来石纤维,例如来自3M的Nextel312或Nextel610纤维;γ-氧化铝+莫来石+非晶SiO2纤维,例如来自3M的Nextel440纤维;γ-氧化铝+非晶SiO2纤维,例如来自3M的Nextel550纤维;石英纤维,例如可得自Saint Gobain;e-玻璃或s-玻璃纤维;硼硅酸盐纤维,例如可得自Mo-SiC Corporation;玄武岩纤维,例如可得自Albarrie;硅灰石纤维,例如可得自Fibertec;等等。
所述无机填充剂粒子可以反而或另外包括纵横比小于10、优选小于2的粒子。这些无机填充剂粒子不同于并且不包括所述胶结剂组合物的无机粘合剂组分。
可以存在无机纤维和低纵横比的无机填充剂粒子的混合物。
所述集料中无机填充剂粒子可以占胶结剂中固体的约30至90重量%。优选的量是所述固体的50至85重量%并且更优选的量是所述固体的60至80重量%。如之前提到,组合物中的“固体”是焙烧步骤完成之后残留的那些无机材料。在大多数情况下,所述固体将由所述无机填充剂粒子和所述无机粘合剂构成。载液和有机材料(包括所述有机聚合物粒子)通常在焙烧步骤期间从胶结剂中损失。因此“固体”不包括任何量的那些材料。
所述胶结剂组合物还包括载液。载液和无机粘合剂的混合物形成糊料或粘性流体,所述无机填充剂粒子和所述有机聚合物粒子分散在其中。所述胶结剂组合物的流体或半流体本质允许它容易施加并与底下的蜂窝充分粘附直到焙烧步骤完成。载液可以是,例如,水、或所述无机粘合剂、无机填充剂粒子和有机聚合物粒子可分散在其中的有机液体。合适的有机液体包括醇、二醇、酮、醚、醛、酯、羧酸、羧酸氯化物、酰胺、胺类、腈、硝基化合物、硫化物、亚砜、砜等等。烃,包括脂族、不饱和脂族(包括烯烃和炔烃)和/或芳烃,是有用的载液。优选地,所述载液是醇、水或其组合。使用醇时,优选甲醇、丙醇、乙醇或其组合。水是最优选的载液。
所述胶结剂组合物含有足够的载液以湿润所述粘合剂粒子并产生糊料或粘性流体,所述无机填充剂粒子和所述有机聚合物粒子分散在其中。有效布氏粘度,利用#6转子以5rpm在25℃下测量,通常为至少约5、10、25、50、75或甚至100Pa·s。所述胶结剂组合物可以表现出剪切变稀行为,使得它的粘度在较高的剪切下变得较低。所述胶结剂组合物中载液的总量(包括可以随所述粘合剂和/或有机聚合物粒子一起带入的任何载液)通常是整体组合物的约25重量%至最多约90重量%。优选的载液量是整体组合物的40至70重量%。
有机聚合物粒子可以占所述胶结剂组合物总重量的约0.5至约85、优选约1至约10并更优选1至5%。所述有机聚合物粒子适合地具有至少10纳米、优选至少25纳米的粒度。所述有机聚合物粒子优选不大于约100微米,并更优选不大于约10微米。尤其优选的粒度是约25至250纳米。
有机聚合物粒子可以是可分散在载液中但不是溶解在其中的任何有机聚合物。所述聚合物可以是非交联的、交联的或支化的。合适的聚合物的例子包括,例如,丙烯酸和/或甲基丙烯酸酯类的聚合物和共聚物;羟烷基丙烯酸酯和/或甲基丙烯酸酯的聚合物,丙烯酰胺的聚合物和共聚物;n-羟甲基丙烯酰胺的聚合物和共聚物;乙烯基芳族单体例如苯乙烯、α-甲基苯乙烯、乙基苯乙烯、二甲基苯乙烯、叔丁基苯乙烯、乙烯基萘、甲氧基苯乙烯、氰基苯乙烯、乙酰基苯乙烯、一氯苯乙烯、二氯苯乙烯、其它卤代苯乙烯等的聚合物和共聚物;丙烯腈的聚合物和共聚物;乙酸乙烯酯的聚合物和共聚物;各种聚烯烃,包括各种聚乙烯(例如低密度聚乙烯(LDPE),线性低密度聚乙烯(LLDPE),高密度聚乙烯(HDPE),基本线性聚乙烯,聚丙烯,聚丁烯,乙烯-丙烯共聚物,乙烯-更高级α-烯烃共聚物,乙烯-丙烯-共轭二烯三元共聚物等等;丁二烯的聚合物和共聚物;苯乙烯-丁二烯共聚物;聚氨酯;聚氨酯-脲;乙烯基氯和/或偏氯乙烯的聚合物和共聚物;不饱和羧酸例如丙烯酸、甲基丙烯酸、衣康酸和富马酸的聚合物和共聚物,等等。
有机聚合物粒子方便提供成胶乳的形式,即在液相中的分散体。在这种情况下,液相通常将形成所述胶结剂组合物的全部或一部分载液。所述有机聚合物粒子可以是乳液聚合方法的产物。或者,所述有机聚合物粒子可以在熔融分散方法中、或通过将粉末粒子分散在液相中而制造。胶乳适合地含有约5至70、优选30至65重量%的分散的有机聚合物粒子。优选的胶乳的pH为至少7,更优选至少8,最多约10,优选最多约9.5。
合适的胶乳及其制备方法的例子描述于USP3,404116,3,399,080、6,720,385和6,753,355;以及WO01/055237、WO01/088007、WO08/077118、WO07/078536和WO09/045731中。
除了所述无机粘合剂、无机填充剂粒子、有机聚合物粒子和载液之外,所述粘固剂还可以含有其他有用组分。有机粘合剂或增塑剂可以为所述胶结剂组合物提供所希望的流变性质,因此优选存在。所述粘合剂不以离散粒子的形式存在,并优选溶解在载液中。合适的粘合剂和有机增塑剂的例子包括纤维素醚,例如甲基纤维素、乙基纤维素、羟丙基甲基纤维素、羟丙基纤维素、羧甲基纤维素等;聚乙二醇,脂肪酸,脂肪酸酯等等。
其它任选的组分包括分散剂、反絮凝剂、絮凝剂、消泡剂、润滑剂和防腐剂,例如在Principles of Ceramic Processing(J.Reed,John Wileyand Sons,NY,1988)的10-12章引言中描述的那些。所述胶结剂组合物还可以含有一种或多种致孔剂。致孔剂是专门添加以在表皮被加热形成非晶相之后在所述表皮中产生孔隙的材料。通常,它们是在加热或焙烧步骤期间分解、蒸发或以某些方式挥发从而留下空隙但不熔化或形成膜的微粒。例子包括面粉、木粉、碳微粒(非晶或石墨的)、坚果壳粉或其组合。
所述胶结剂组合物可以通过以任何方便的顺序简单混合前述的组分而制备。
所述胶结剂组合物施加于所述蜂窝的至少一个多孔表面。施加所述胶结剂组合物的方式不是关键的,可以以需要的厚度施加所述组合物的任何合适的方法都是适当的。所述胶结剂可以手工施加或通过使用各种类型的机械设备施加。所述胶结剂组合物可以在低于一大气压力下施加,以促进在施加过程期间除去载液。
如果所述胶结剂组合物用来将多个部件(例如多个蜂窝)组装成更大的组件,所述胶结剂以任何方便的方式施加于待组装的一个或多个所述部件的表面,然后所述部件利用介入所述部件相邻表面之间的胶结剂组合物来接合。经焙烧后,在所述部件之间形成干的胶结剂接缝并将它们粘附在一起。
如果所述胶结剂组合物待用于在蜂窝(或包含蜂窝的组件)上形成外周表皮,则所述组合物被施加于所述蜂窝外周的至少一部分上。这样制造的陶瓷蜂窝通常具有外周“表皮”,它可以仅仅是所述蜂窝结构的外周巢室的外巢室壁。通常可优选在根据本发明施加替换表皮之前除去这样的表皮。至少所述蜂窝的外周巢室的外壁被除去。更通常地,除去所述“表皮”只是更通用的成形过程的一部分,其中所述陶瓷蜂窝的外部部分被除去以使其横截面的形状和尺寸达到需要的规格。从陶瓷蜂窝除去外周部分的这个步骤暴露了在除去步骤完成之后留在所述蜂窝外周上的轴向延伸的巢室的内部。所述胶结剂组合物然后施加于所述蜂窝的新暴露的外周的至少一部分上。
所述蜂窝的外周通常不光滑,并且在大多数情况下所述蜂窝外周周围的一定比例的轴向延伸的巢室将在施加所述胶结剂组合物以形成表皮之前开放。所述胶结剂组合物通常将以填充那些开放的巢室并且形成稍光滑的外表面的这样的方式来施加。因此,所述表皮的厚度通常将变化。在它的最薄点,施加的表皮应该为至少1mm厚,并且可以多达25mm厚。
所述胶结剂组合物在它施加于所述蜂窝之后被焙烧。所述焙烧步骤从所述胶结剂除去载液、有机聚合物粒子和任何其它有机材料(包括任何致孔剂)。无机粘合剂在焙烧步骤期间形成粘合相。所述粘合相将无机粒子粘合在一起,并将施加的胶结剂层与底下的蜂窝结构相粘合。
焙烧步骤在至少600℃的温度下进行,并且可以在低于所述蜂窝软化或降解的任何较高的温度下进行。焙烧温度可以为至少800℃。焙烧温度超过1500℃通常不需要,并且1200℃或更低的焙烧温度是优选的。在优选的焙烧方案中,所述蜂窝和施加的胶结剂组合物以不高于20℃/分钟、优选不高于10℃/分钟并且还更优选不高于5℃/分钟的速率从环境温度加热直至焙烧温度。逐渐加热速率意图是帮助防止热冲击并且还为了提供除去载液和任何有机材料(包括所述聚合物粒子)的时间。如果需要,所述组件可以在一种或多种中等温度下或在最高温度下保持一段时间。这对于例如以一定的预定顺序除去载液、有机聚合物粒子、有机粘合剂和/或致孔剂以允许一些化学反应发生、或为了一些其它原因,可能是所期望的。
焙烧步骤期间可发生的化学反应的例子是从所述胶结剂组合物的组分产生莫来石。形成莫来石需要在所述胶结剂组合物中存在一种或多种硅和铝酸盐原子源。胶态二氧化硅和胶态铝当然分别是硅和铝原子源。如果胶态二氧化硅独自用于形成粘合剂相,则所述胶结剂组合物必须含有一些另外的铝原子源。这种源通常是无机填充剂粒子,其除了必要的铝原子之外还可以含有硅原子。类似地,如果胶态氧化铝独自用于形成粘合剂相,则所述胶结剂组合物必须含有一些另外的硅原子源,其同样通常将是所述无机填充剂粒子。在该第二种情况中,所述无机填充剂除了需要的硅原子之外,还可以含有铝原子。这些硅和铝原子源在所述焙烧步骤期间能够反应形成莫来石。这些源材料可以形成针状莫来石,如果在氟源存在下加热(通常在600至900℃温度下)形成氟黄玉,然后进一步加热到至少900℃、优选至少1000℃并更优选至少1100℃的温度以分解所述氟黄玉并形成针状莫来石的话。氟源可以是,例如SiF4、AlF3、HF、Na2SiF6、NaF、NH4F、氟化聚合物例如氟化聚乙烯或聚四氟乙烯、或甚至针状莫来石蜂窝中含有的残余氟、或其任何两种或更多种的一些混合物。
可替代地或另外,所述焙烧步骤可以与制备底下的过滤器和/或最终部件所需的一些其它热处理步骤同时进行。例如,针状莫来石蜂窝倾向于含有一些残余的氟。氟的量可以占所述针状莫来石重量的0.5至约3重量%。在常规方法中,这种残余的氟通过将所述蜂窝优选在空气中或在氧气存在下加热到至少1200℃、优选至少1400℃的温度来除去。本发明的焙烧步骤可以与从针状莫来石蜂窝除去残余氟的同时进行。
焙烧的胶结剂的弹性模量优选显著低于底下的陶瓷蜂窝的弹性模量。焙烧的胶结剂的弹性模量可以例如在所述蜂窝中陶瓷材料的弹性模量的3至35%范围内。据认为,这种较低的模量有助于降低所述蜂窝在再生期间的热机械应力。焙烧的胶结剂的模量可如下评价:从所述胶结剂组合物形成8mm X4mm X40mm试验棒,焙烧所述试验棒并利用Grindosonic脉冲激发设备按照ASTM Standard C1259-98——通过脉冲激发振动测量高级陶瓷的动态杨氏模量、剪切模量和泊松比率的标准试验方法(Standard Test Method for Dynamic Young's modulus,ShearModulus,and Poisson's Ratio for Advanced Ceramics by impulse excitationof Vibration)来测量模量。
焙烧步骤期间胶结剂组合物中存在有机聚合物粒子减少了所述胶结剂渗透到底下的蜂窝结构的壁中。这进而减少巢室堵塞,导致在使用和/或再生时通过所述过滤器的压降较小和蜂窝内的温度梯度较小。还已经发现,胶结剂组合物中存在有机聚合物粒子减少了抗热冲击性损失,抗热冲击性损失在常规胶结剂组合物施加于陶瓷蜂窝并焙烧时是经常看到的。
有机聚合物粒子提供这些益处的机制不完全了解。虽然本发明不限于任何理论,但一种解释是所述有机聚合物粒子机械阻塞蜂窝结构壁中的孔隙,提供了所述胶结剂组合物的无机粘合剂部分渗透的物理屏障。还可能是所述有机聚合物粒子也许部分由于pH效应而与一部分或所有的无机粘合剂粒子结合、包覆和/或团聚,并抑制它们的流动性和从而抑制它们渗透入陶瓷蜂窝的孔隙中的能力。添加胶乳形式的聚合物粒子可以增加胶结剂组合物的粘度,从而妨碍它渗透入蜂窝壁的孔隙中。所述有机聚合物粒子在所述施加和/或焙烧步骤期间可以凝结和/或形成短效(fugitive)膜,这再次完全或部分阻断了所述胶结剂流入孔隙中。尽管存在有机聚合物粒子,但所述胶结剂组合物仍然保持其有效形成与所述蜂窝的强胶粘结合的能力。
根据本发明产生的蜂窝可用作微粒过滤器,特别是用于从动力设备(活动或固定的)排气中除去微粒物质。这种类型的具体应用是内燃机、尤其是柴油发动机的烟尘过滤器。
功能材料可以在施加和焙烧所述胶结剂组合物之前或之后,利用各种方法施加于所述蜂窝。所述功能材料可以是有机或无机的。无机功能材料,特别是金属和金属氧化物,是所关心的,因为它们中许多具有期望的催化性质、起吸附剂的作用或执行一些其它需要的功能。将金属或金属氧化物引入到所述复合体上的一种方法是通过用金属的盐或酸溶液浸渍所述蜂窝,然后加热或以其它方式除去溶剂,以及如有必要,煅烧或以其它方式分解所述盐或酸以形成想要的金属或金属氧化物。
因此,例如,经常施加氧化铝涂层或其它金属氧化物的涂层,以提供可以在其上沉积催化或吸附材料的较高表面积。通过用胶态氧化铝浸渍所述蜂窝,然后,通常通过使气体通过所述浸渍体进行干燥,来沉积氧化铝。这种程序可以根据需要进行重复,以沉积需要的氧化铝量。其它陶瓷涂层例如二氧化钛可以通过类似的方式施加。
金属例如钡、铂、钯、银、金等可以通过用所述金属的可溶盐例如硝酸铂、氯化金、硝酸铑、四氨基硝酸钯、甲酸钡浸渍所述蜂窝(其内壁优选涂有氧化铝或其它金属氧化物),然后干燥并优选煅烧,从而沉积在所述复合体上。用于动力设备排气流、尤其是用于汽车的催化转化器可以用这种方式从所述具有表皮的蜂窝制备。
将各种无机材料沉积到蜂窝结构上的合适的方法描述于例如US205/0113249和WO2001045828中。这些方法通常与本发明的具有表皮的蜂窝有关。
在一种特别优选的实施方式中,氧化铝和铂、氧化铝和钡、或氧化铝、钡和铂可以在一个或多个步骤中沉积到所述蜂窝上,以形成能够从动力设备排气、例如从汽车发动机同时除去微粒例如烟尘、NOx化合物、一氧化碳和烃的过滤器。
提供以下实施例是为了说明本发明,而不是想要限制其范围。全部份数和百分数都按重量计,除非另外指出。
实施例1
胶结剂例1如下制备:39.9份球磨的硅酸铝锆纤维(Fiberfrax LongStaple Fine纤维,出自Unifrax LLC,Niagara Falls,NY)、12.8份胶态氧化铝(AL20SD,出自Nyacol Nano technologies,Inc.,Ashland,Maine)、38.5份水、1.9份甲基纤维素(Methocel A15LV,可得自The Dow ChemicalCompany)、1.9份聚乙二醇400(出自Alfa Aesar,Ward Hill,Massachusetts)和5.0份细粒度的45%固体丙烯酸胶乳(Neocar850,出自The Dow Chemical Company,pH约8.5)混合形成均匀混合物。所述丙烯酸胶乳向所述混合物提供大约2.25重量份分散的70nm丙烯酸类聚合物粒子。
向一部分胶结剂例1添加红色的食品色素。着色的混合物然后涂布在陶瓷蜂窝上。所述蜂窝是10巢室X10巢室X3英寸(7.6cm)针状莫来石,每平方英寸具有200个巢室(31巢室/平方厘米)。让施加的胶结剂层空气干燥,然后切开所述蜂窝以检查所述胶结剂组合物扩散到所述蜂窝结构中的程度。来自食用染料的红颜色延伸到所述蜂窝结构中的距离等于大约巢室宽度的一半。
利用3051压力变送器(可得自Rosemount,Inc.,Eden Prairie,MN)在100/min空气流速的流速下,测量通过另一个类似(但是未涂层的)蜂窝节段的压降。然后将一部分胶结剂例1涂布到所述同一蜂窝节段的外周表面上,所述涂层蜂窝在1100℃下焙烧。通过所述涂层和焙烧的蜂窝的压降只比通过所述未涂层的蜂窝的压降高7%。
实施例2和比较样品A
胶结剂例2如下制备:38.9份球磨的硅酸铝锆纤维(Fiberfrax LongStaple Fine纤维,出自Unifrax LLC,Niagara Falls,NY)、12.5份胶态氧化铝(AL20SD,出自Nyacol Nano technologies,Inc.,Ashland,Maine)、37.5份水、1.8份甲基纤维素(Methocel A15LV,可得自The Dow ChemicalCompany)、1.8份聚乙二醇400(出自Alfa Aesar,Ward Hill,Massachusetts)和7.5份细粒度的45%固体丙烯酸胶乳(Neocar850,出自The Dow Chemical Company)混合形成均匀混合物。所述丙烯酸胶乳向所述混合物提供大约3.4重量份分散的70nm丙烯酸类聚合物粒子。
向所述混合物添加红色食品色素。着色的混合物然后如实施例1所述涂布在陶瓷蜂窝上并空气干燥。所述蜂窝然后如实施例1所述切开。几乎没有来自食用染料的红颜色渗透入所述蜂窝中。
如实施例1所述测量通过另一个蜂窝节段的压降。所述节段然后如实施例1所述涂布所述胶结剂组合物并焙烧,再次测量通过所述涂层过滤器的压降。通过所述涂层蜂窝的压降只比通过未涂层的蜂窝的压降高2%。
另外,一部分胶结剂例2被用来将九个3"X3"X8"(7.6cm X7.6cm X22.9cm)蜂窝节段胶结成更大的正方形组件,所述组件的正方形横截面一边为九英寸(22.9cm)并且和长度为八英寸(20.4cm)。这些蜂窝节段是针状莫来石并具有200巢室/平方英寸(31巢室/cm2)。组装的蜂窝焙烧到1100℃的温度并在冷却到室温后机械加工,产生直径为九英寸(22.9cm)的圆柱形蜂窝。更多的胶结剂例2施加于所述机械加工的蜂窝的外周表面以形成表皮。该表皮在1100℃下焙烧。
所述具有表皮的蜂窝结构然后进行热试验台(thermal bench)试验,其中热空气通过所述结构以产生热机械应力。所述热空气以100标准立方英尺/分钟(0.47m3/秒)的速率吹过所述结构。空气温度以200℃/分钟的速率增加,直到空气温度达到700℃。植入的热电偶测量外周表皮处和距表皮约10mm的通道中的蜂窝温度,以评价以这种加热方案形成的温度梯度。该温差是64℃。类似地,植入的热电偶测量接缝和距所述接缝10mm的通道中的温度,作为所形成的温度梯度的另一个指标。该温差是68℃。通过该结构的压降是107Pa。
比较胶结剂样品A通过混合以下成分而制备:42.0份球磨的硅酸铝锆纤维,13.5份胶态氧化铝,40.5份水,2.0份甲基纤维素,和2.0份聚乙二醇400。比较胶结剂样品A不含聚合物粒子。
向一部分比较胶结剂样品A添加红色的食品色素,然后将所述着色的混合物如前所述涂布到陶瓷蜂窝上并空气干燥。然后当所述蜂窝被切开时,看到来自所述食用染料的红颜色渗透入所述蜂窝的距离大于一个巢室的宽度。这些结果当与胶结剂例2相比较时,表明存在有机聚合物粒子非常显著地减少了所述胶结粘合剂材料渗透通过所述蜂窝的多孔壁。
另一个类似的蜂窝节段以与实施例1和2所述的相同方式涂布另一部分比较胶结剂样品A。如前所述,在焙烧后测量未涂层的蜂窝节段和涂层节段的压降。通过涂有比较胶结剂样品A的蜂窝的压降比通过未涂层的蜂窝的压降高13%。该结果,与用胶结剂例2得到的结果结合起来,表明存在有机聚合物粒子导致明显减少了通过蜂窝结构的压降。
其他部分的比较胶结剂样品A以与胶结剂例2所述的同样方式用于形成分段式和具有表皮的蜂窝结构。所生成的具有表皮的蜂窝结构在上面描述的热试验台试验中评价。表皮和距所述表皮10mm的通道之间的温度梯度是87℃;而且接缝和距所述接缝10mm的通道之间的温度梯度是139℃。这些温度梯度比胶结剂例2用于形成接缝和表皮时所见的温度梯度高许多。在胶结剂例2中存在所述胶乳可看出降低了在所述分段和具有表皮的蜂窝结构中形成的温度梯度。通过该结构的压降是116Pa,或比利用胶结剂例2作为接缝和表皮材料制造的结构的压降高约8%。
实施例3和比较样品B
胶结剂例3如下制备:40.6份球磨的硅酸铝锆纤维(Fiberfrax LongStaple Fine纤维,出自Unifrax LLC,Niagara Falls,NY)、13.0份胶态氧化铝(Dispal14N4-80,出自Sasol North America,Inc.,Houston,Texas)、39.1份水、1.9份甲基纤维素(Methocel A15LV,可得自The Dow ChemicalCompany)、1.9份聚乙二醇400(出自Alfa Aesar,Ward Hill,Massachusetts)和3.5份细粒度的45%固体丙烯酸胶乳(Neocar850,出自The Dow Chemical Company)混合形成均匀混合物。所述丙烯酸胶乳向所述混合物提供大约1.6重量份分散的70nm丙烯酸类聚合物粒子。
向一部分胶结剂例3添加红色食品色素。着色的混合物然后如实施例1所述涂布在陶瓷蜂窝上并空气干燥。所述蜂窝然后如实施例1所述切开。几乎没有来自食用染料的红颜色渗透进入所述蜂窝中。
当另一个同样的蜂窝节段如实施例1所述涂布胶结剂例3并焙烧时,通过所述过滤器的压降与未涂层的蜂窝相比只增加3%。
比较胶结剂样品B如下制备:42.0份球磨的硅酸铝锆纤维(FiberfraxLong Staple Fine纤维,出自Unifrax LLC,Niagara Falls,NY)、13.5份胶态氧化铝(Dispal14N4-80,出自Sasol North America,Inc.,Houston,Texas)、40.5份水、2.0份甲基纤维素(Methocel A15LV,可得自The DowChemical Company)和2.0份聚乙二醇400(出自Alfa Aesar,Ward Hill,Massachusetts)混合形成均匀混合物。如前所述,向一部分所述混合物添加红色的食品色素,然后将所述混合物涂布到陶瓷蜂窝上并空气干燥。红颜色渗透入所述蜂窝的距离等于大约一个巢室的宽度,这明显差于当胶结剂例3用来涂布所述蜂窝时所看到的。
当另一个同样的蜂窝节段涂布比较胶结剂样品B并焙烧时,通过所述蜂窝的压降与未涂层的蜂窝相比增加了约10%。
Claims (15)
1.用于将胶结层施加到多孔陶瓷蜂窝结构上的方法,所述方法包括以下步骤:(a)向陶瓷蜂窝的至少一个多孔表面施加胶结剂组合物,所述陶瓷蜂窝包含由相交的多孔壁限定的多个轴向延伸的巢室,和(b)焙烧所述蜂窝和胶结剂组合物,其中所述胶结剂组合物含有至少一种无机粘合剂、至少一种无机填充剂、载液和分散在所述载液中的粒度为约10纳米至100微米的有机聚合物粒子。
2.权利要求1的方法,其中所述胶结剂组合物含有0.5至85重量%的所述有机聚合物粒子。
3.权利要求2的方法,其中所述胶结剂组合物含有1至5重量%的所述有机聚合物粒子。
4.任一前述权利要求的方法,其中所述有机聚合物粒子以胶乳的形式提供。
5.权利要求4的方法,其中所述胶乳是乳液聚合的产物。
6.权利要求4或5的方法,其中所述胶乳的pH为至少7。
7.权利要求6的方法,其中所述胶乳的pH为8至9.5。
8.任一前述权利要求的方法,其中所述有机聚合物粒子具有至少25纳米的粒度。
9.权利要求8的方法,其中所述有机聚合物粒子具有25微米或更小的粒度。
10.权利要求8的方法,其中所述有机聚合物粒子具有25至250纳米的粒度。
11.任一前述权利要求的方法,其中所述无机粘合剂包括胶态二氧化硅、胶态氧化铝、或其混合物。
12.任一前述权利要求的方法,其中所述载液包括水、醇或其混合物。
13.任一前述权利要求的方法,其中所述胶结剂层在所述陶瓷蜂窝上形成外周表皮。
14.任一前述权利要求的方法,其中所述胶结剂层将陶瓷蜂窝与另外的陶瓷蜂窝相粘附。
15.任一前述权利要求的方法,其中所述焙烧步骤在800℃至1500℃的温度下进行。
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US201161510811P | 2011-07-22 | 2011-07-22 | |
US61/510,811 | 2011-07-22 | ||
PCT/US2012/044381 WO2013015932A1 (en) | 2011-07-22 | 2012-06-27 | Process for producing cemented and skinned ceramic honeycomb structures |
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