CN110382080B - 蜂窝过滤器 - Google Patents

蜂窝过滤器 Download PDF

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Publication number
CN110382080B
CN110382080B CN201880015092.7A CN201880015092A CN110382080B CN 110382080 B CN110382080 B CN 110382080B CN 201880015092 A CN201880015092 A CN 201880015092A CN 110382080 B CN110382080 B CN 110382080B
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honeycomb filter
port hole
wall portion
honeycomb
end portion
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CN201880015092.7A
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CN110382080A (zh
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后藤真之助
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Ibiden Co Ltd
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Ibiden Co Ltd
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    • B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
    • B01J23/54—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
    • B01J23/56—Platinum group metals
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    • B01D39/14—Other self-supporting filtering material ; Other filtering material
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Abstract

蜂窝过滤器被用于微粒的捕集，其具备由以二氧化铈‑氧化锆复合氧化物和无机粘结剂作为构成成分的基材构成的壁部(13)。壁部(13)在将由压汞法测定的气孔径和log微分细孔容积分别作为横轴和纵轴的气孔径分布中在气孔径为0.01μm以上且小于1μm的范围具有峰、并且在气孔径为1μm以上50μm以下的范围具有峰。

Description

蜂窝过滤器
技术领域
本发明涉及用于微粒的捕集的蜂窝过滤器。
背景技术
专利文献1中，作为用于微粒的捕集的蜂窝过滤器，公开了一种由碳化硅构成的蜂窝过滤器。专利文献2中公开了一种尾气净化催化剂，其是使贵金属负载于包含二氧化铈-氧化锆复合氧化物颗粒的整体基材而成的。其中记载了，通过利用二氧化铈-氧化锆复合氧化物颗粒构成基材，可减小热容量、提高整体基材的温度，提高催化剂的预热性能。
现有技术文献
专利文献
专利文献1：国际公开第2006/041174号
专利文献2：日本特开2015-85241号公报
发明内容
发明所要解决的课题
另外，为了提高专利文献1中公开的蜂窝过滤器的预热性能，作为蜂窝过滤器的壁部，认为可采用专利文献2中公开的包含二氧化铈-氧化锆复合氧化物颗粒的基材。但是，专利文献2中公开的包含二氧化铈-氧化锆复合氧化物颗粒的基材中，由于包含微粒的气体几乎无法通过壁部，因此其不适合作为捕集微粒的蜂窝过滤器的壁部。其原因在于，尽管碳化硅颗粒通过再结晶而在颗粒间形成气孔(pore)，但由于二氧化铈-氧化锆复合氧化物颗粒利用无机粘结剂进行结合，因此未能在颗粒间形成气体可通过的适当尺寸的气孔。另外，还考虑了将由碳化硅等基材构成的壁部利用二氧化铈-氧化锆复合氧化物被覆的构成，但由于二氧化铈-氧化锆复合氧化物的负载量被限定于可被覆壁部的范围，因此尾气净化性能的提高效果小。此外，由于制成被覆于基材的结构而使得蜂窝过滤器的重量也增加，因此预热性能降低。本发明是鉴于这样的情况而完成的，其目的在于提供预热性能优异的蜂窝过滤器。
用于解决课题的手段
用于解决上述课题的本发明的蜂窝过滤器是用于微粒的捕集的蜂窝过滤器，其要点在于，该蜂窝过滤器具备由以二氧化铈-氧化锆复合氧化物和无机粘结剂作为构成成分的基材构成的壁部，上述壁部在将由压汞法测定的气孔径和log微分细孔容积分别作为横轴和纵轴的气孔径分布中在气孔径为0.01μm以上且小于1μm的范围具有峰、并且在气孔径为1μm以上50μm以下的范围具有峰。
根据该构成，通过使蜂窝过滤器具备由以二氧化铈-氧化锆复合氧化物作为构成成分的基材构成的壁部，与在由碳化硅等基材构成的壁部被覆二氧化铈-氧化锆复合氧化物的构成相比，在为相同的二氧化铈-氧化锆复合氧化物的含量时更能够减小壁部的热容量。另外，作为处理对象的气体通过在气孔径为0.01μm以上且小于1μm的范围具有峰的气孔而能够效率良好地扩散到壁部的内部。由此可提高扩散在壁部的内部的气体的净化性能。另外，通过存在有在气孔径为1μm以上50μm以下的范围具有峰的气孔，壁部的气体透过性提高，因此在具有作为捕集微粒的过滤器的功能的同时还能够将压力损失抑制得较低。此处，“预热性能”是指蜂窝过滤器升高到可得到充分的净化性能的温度的容易性。即，在像本发明的蜂窝过滤器这样每单位体积的重量小、净化性能高时，“预热性能”良好。
本发明的蜂窝过滤器中，上述壁部优选具有贯穿该壁部的直径为1μm以上50μm以下的线状的气孔。根据该构成，气体容易通过贯穿壁部的气孔而穿过壁部，因此可适宜地提高壁部的气体透过性。
本发明的蜂窝过滤器的基材优选包含氧化铝作为构成成分。根据该构成，通过包含氧化铝作为基材的构成成分，在使催化剂负载于基材时能够使其高分散，能够提高作为处理对象的气体的净化性能。另外，能够提高高温状态下的壁部的机械强度。
本发明的蜂窝过滤器中，优选催化剂被负载于上述基材。根据该构成，蜂窝过滤器不仅能够发挥出捕集微粒的功能，而且还能够发挥出作为处理对象的气体的净化作用等基于催化剂的功能。
本发明的蜂窝过滤器中，上述催化剂优选为贵金属。二氧化铈-氧化锆复合氧化物具有作为促进由贵金属构成的催化剂的催化作用的助催化剂的功能。因此，本发明的蜂窝过滤器通过与由贵金属构成的催化剂组合而能够发挥出高催化作用。
本发明的蜂窝过滤器优选具有多个孔道，该多个孔道被上述壁部分隔、并且从上述蜂窝过滤器的作为一端侧的第1端部延伸至作为另一端侧的第2端部。上述孔道优选具备：上述第1端部侧的端部开放、上述第2端部侧的端部密封的第1孔道；与上述第1孔道相邻且上述第1端部侧的端部密封、上述第2端部侧的端部开放的第2孔道；以及与上述第1孔道和上述第2孔道中的至少一者相邻且上述第1端部侧的端部和上述第2端部侧的端部这两个端部开放的第3孔道。根据该构成，能够利用第1孔道与第2孔道间的壁部捕集微粒。另外，通过具备第1端部侧的端部和第2端部侧的端部这两个端部开放的第3孔道，能够降低蜂窝过滤器的压力损失。
发明的效果
根据本发明，能够提供预热性能优异的蜂窝过滤器。
附图说明
图1是蜂窝过滤器的立体图。
图2是图1的2-2线截面图。
图3是示出实施例的壁部的气孔径分布的曲线图。
图4是示出比较例的壁部的气孔径分布的曲线图。
图5是压力损失测定装置的示意图。
具体实施方式
以下对本发明的一个实施方式进行说明。
如图1所示，本实施方式的蜂窝过滤器10具备筒状的周壁11、以及将周壁11的内部分隔成多个孔道S的截面为蜂窝形状的分隔壁12。各孔道S从周壁11的轴向的一端侧延伸至另一端侧、即从蜂窝过滤器10的作为一端侧的第1端部延伸至作为另一端侧的第2端部。壁部13由周壁11和分隔壁12构成。蜂窝过滤器10的孔道结构没有特别限定，例如，可以形成分隔壁12的壁厚为0.1～0.7mm、每1cm2的孔道密度为15.5～124个孔道的孔道结构。需要说明的是，上述“0.1～0.7mm”是指“0.1mm以上0.7mm以下”，上述“15.5～124个孔道”是指“15.5个孔道以上124个孔道以下”。即，本说明书中，“A～B”是指“A以上B以下”。
壁部13由以二氧化铈-氧化锆复合氧化物(以下也称为“CZ复合氧化物”)、无机粘结剂和氧化铝作为构成成分的基材形成。即，构成壁部13的基材中包含CZ复合氧化物、无机粘结剂和氧化铝。并且，在构成基材的颗粒的表面负载有催化剂。
构成本发明的蜂窝过滤器的基材的CZ复合氧化物中，二氧化铈优选包含10质量％以上、更优选包含20质量％以上。另外，二氧化铈优选包含70质量％以下、更优选包含60质量％以下。通过包含10质量％以上二氧化铈，尾气中的氧的吸收释放能力提高；通过使该含量为70质量％以下，热耐久性提高。
CZ复合氧化物可以进一步包含选自除铈以外的稀土元素中的元素。作为除铈以外的稀土元素，可以举出钪(Sc)、钇(Y)、镧(La)、镨(Pr)、钕(Nd)、钐(Sm)、钆(Gd)、铽(Tb)、镝(Dy)、镱(Yb)、镥(Lu)等。
基材中的CZ复合氧化物的含量优选为15～60质量％。
作为上述无机粘结剂，例如可以使用氧化铝溶胶、硅溶胶、二氧化钛溶胶、水玻璃、海泡石、凹凸棒石、膨润土、勃姆石。基材中的无机粘结剂的含量没有特别限定，优选相对于基材含有10～30质量％。
作为上述氧化铝，优选包含氧化铝颗粒。在包含氧化铝颗粒时，容易分散负载上述作为催化剂使用的例如贵金属，并且能够提高壁部13的机械强度。作为氧化铝颗粒的种类没有特别限定，优选使用θ相的氧化铝(以下也称为“θ-氧化铝”)、γ相的氧化铝(以下也称为“γ-氧化铝”)。θ-氧化铝即使被暴露于1000℃左右的高温时其相变也被抑制，因此通过将θ-氧化铝用于基材的构成成分，高温状态下的蜂窝过滤器10的机械强度提高。由于γ-氧化铝的比表面积大，因此能够将作为催化剂使用的贵金属高分散。基材中的氧化铝颗粒的含量没有特别限定，优选相对于基材含有15～60质量％。
基材中可以包含CZ复合氧化物、无机粘结剂、氧化铝以外的其他成分。作为其他成分，例如可以举出热膨胀系数小于CZ复合氧化物和氧化铝的颗粒(以下也称为“低热膨胀系数颗粒”)等其他无机颗粒。
在含有低热膨胀系数颗粒作为其他成分的情况下，能够减小基材的热膨胀系数，因此蜂窝过滤器10的耐热冲击性提高。作为低热膨胀系数颗粒，例如可以举出堇青石、钛酸铝、铝硅酸锂盐系材料的颗粒。作为铝硅酸锂盐系材料，例如可以举出β-锂辉石、β-锂霞石。低热膨胀系数颗粒的含量没有特别限定，优选相对于基材含有5～30质量％。
作为负载于基材的催化剂，可以举出贵金属、碱金属(元素周期表1族)、碱土金属(元素周期表2族)、稀土元素(元素周期表3族)、过渡金属元素，优选贵金属。作为贵金属，例如可以举出铂、钯、铑等铂族金属。贵金属的负载量没有特别限定，相对于蜂窝过滤器10的表观体积(L)优选为0.1～20g/L、更优选为0.5～15g/L。
如图2所示，多个孔道S中，特定的几个孔道S的端部被密封部14密封。即，蜂窝过滤器10中具备第1孔道S1和第2孔道S2，第1孔道S1中，蜂窝过滤器10的第1端部侧(一端侧)的端部开放，第2端部侧(另一端侧)的端部密封；第2孔道S2与第1孔道S1相邻，第1端部侧的端部密封、第2端部侧的端部开放。由于第1孔道S1和第2孔道S2中，相互不同侧的端部被密封，因此如图2中的箭头所示，在蜂窝过滤器10的一端侧流入到第1孔道S1内的气体通过第1孔道S1与第2孔道S2之间的壁部13的内部而流入到第2孔道S2内，之后在蜂窝过滤器10的另一端侧流出到蜂窝过滤器10的外部。此时，气体中含有的微粒被捕集到壁部13的第1孔道S1侧的表面。
另外，蜂窝过滤器10可以进一步具备与第1孔道S1和第2孔道S2中的至少一者相邻且蜂窝过滤器10的一端侧的端部和另一端侧的端部这两个端部开放的第3孔道S3。即，多个孔道S中，有数个孔道可以两端部均不密封。在蜂窝过滤器10的一端侧流入到第3孔道S3内的气体可以直接通过相同的第3孔道S3内而在蜂窝过滤器10的另一端侧流出到蜂窝过滤器10的外部。第3孔道S3与第1孔道S1相邻的情况下，在蜂窝过滤器10的一端侧流入到第1孔道S1内的气体也可以通过第1孔道S1与第3孔道S3之间的壁部13的内部而流入到第3孔道S3内，之后在蜂窝过滤器10的另一端侧流出到蜂窝过滤器10的外部。
第3孔道S3的配置位置在与第1孔道S1和第2孔道S2中的至少一者相邻的范围内适宜地选择。例如，如图2所示，可以使蜂窝过滤器10的外周侧的截面积小的孔道S为第3孔道S3。另外，第3孔道S3在全部的孔道S中所占的比例没有特别限定，优选为1/3以下。
图2所示的密封部14的长度T没有特别限定，优选比分隔壁12的壁厚厚。分隔壁12的壁厚为0.1～0.7mm的情况下，密封部14的长度T优选为1～10mm。
接着对蜂窝过滤器10的壁部13的气孔径分布进行说明。
本实施方式的蜂窝过滤器10用于由车辆或建设机械等的内燃机排出的气体中包含的微粒的捕集。因此，蜂窝过滤器10的分隔壁12具有用于使处理对象的气体通过的气孔(pore)。分隔壁12是具有特定的气孔径分布的壁部，如图3所示，将利用压汞法测定的气孔径和log微分细孔容积分别作为横轴和纵轴时，上述特定的气孔径分布在气孔径为0.01μm以上且小于1μm的范围和气孔径为1μm以上50μm以下的范围分别具有峰。在气孔径为0.01μm以上且小于1μm的范围存在的峰来自于在被用于原料中的CZ复合氧化物等的颗粒间的间隙所形成的气孔。在气孔径为0.01μm以上且小于1μm的范围存在的峰数可以仅为1个，也可以为多个。
在气孔径为1μm以上50μm以下的范围存在的峰来自于由后述的蜂窝过滤器10的制造方法形成的气孔。来自于该制造方法的气孔例如形成为贯穿分隔壁12的直径为1μm以上50μm以下的线状。在气孔径为1μm以上50μm以下的范围存在的峰数可以仅为1个，也可以为多个。在气孔径为0.01μm以上且小于1μm的范围存在的气孔与在气孔径为1μm以上50μm以下的范围存在的气孔的比例没有特别限定，以体积比计优选为10：1～1.5：1。
需要说明的是，贯穿分隔壁12的线状的气孔可以通过使用电子显微镜对分隔壁12的断裂面进行观察来确认。在使用电子显微镜观察的直径为1μm以上50μm以下的气孔之中，优选80％以上的气孔为贯穿分隔壁12的线状的气孔。另外，线状气孔的形状可以为直线状、曲线状、折线状中的任一种。
分隔壁12的气孔率没有特别限定，优选为40～80％、更优选为55～75％。密封部14的气孔率没有特别限定，优选为40～80％、更优选为55～75％。分隔壁12的气孔径分布和气孔率可以利用压汞法在接触角为130°、表面张力为485mN/m的条件下进行测定。
接着对本实施方式的蜂窝过滤器10的制造方法进行说明。蜂窝过滤器10通过依序经历以下记载的混合工序、成型工序、密封工序、脱脂工序、烧制工序、负载工序来制造。
(混合工序)
混合工序为将CZ复合氧化物颗粒、无机粘结剂、氧化铝颗粒、有机纤维等原料混合来制作原料混合物的工序。作为CZ复合氧化物颗粒，优选使用二氧化铈与氧化锆的固溶体。二氧化铈与氧化锆的固溶体例如可以如下制备：向溶解有硝酸铈等铈盐和硝酸氧锆等锆盐的水溶液中加入氨水而生成共沉淀物，将所得到的沉淀物干燥后在400～500℃烧制5小时左右，由此制备出该固溶体。
作为原料之一的CZ复合氧化物颗粒的平均粒径没有特别限定，优选为1～10μm、更优选为1～5μm。平均粒径可以利用激光衍射式粒度分布测定装置进行测定。
作为无机粘结剂，可以使用上述无机粘结剂的具体例中的任一种。原料混合物中的无机粘结剂的比例没有特别限定，以固体成分计优选为10～30质量％。
作为氧化铝颗粒，如上所述，可以使用θ-氧化铝颗粒、γ-氧化铝颗粒。原料混合物中的氧化铝颗粒的比例没有特别限定，以固体成分计优选为10～50质量％。氧化铝颗粒的平均粒径没有特别限定，以二次颗粒计优选为1～10μm、更优选为1～5μm。
作为有机纤维，可以使用例如丙烯腈系纤维、聚酯纤维等。有机纤维的尺寸没有特别限定，直径优选为1～50μm、更优选为3～40μm。另外，长度优选为0.1～30mm、更优选为0.1～10mm。原料混合物中的有机纤维的比例没有特别限定，以固体成分计优选为10～50质量％。
上述原料混合物中，可以根据需要添加上述的低热膨胀系数颗粒、或者无机纤维、有机粘结剂、造孔剂、成型助剂、分散介质。
低热膨胀系数颗粒的平均粒径没有特别限定，优选为1～10μm、更优选为1～5μm。
作为构成无机纤维的材料，例如可以举出氧化铝、氧化硅、氧化硅-氧化铝、玻璃。
作为有机粘结剂，例如可以举出甲基纤维素、羧甲基纤维素、羟乙基纤维素、聚乙二醇、酚树脂、环氧树脂。
造孔剂可以为与有机纤维不同的颗粒状，作为这样的造孔剂，可以举出丙烯酸系树脂、焦炭、淀粉。
作为成型助剂，可以举出乙二醇、糊精、脂肪酸、脂肪酸皂、多元醇、表面活性剂。
作为分散介质，可以举出水、苯等有机溶剂、甲醇等醇。
这些原料可以使用公知的混合器或超微磨碎机等进行混合，也可以进一步利用捏合机等进行混炼。
(成型工序)
成型工序是将由混合工序得到的原料混合物进行成型来制作蜂窝成型体的工序。蜂窝成型体按照经过后述的烧制工序中的烧制收缩而成为与蜂窝过滤器10相同的形状的方式例如通过使用挤出模具对原料混合物进行挤出成型并切断成规定的长度来制作。即，通过将构成蜂窝过滤器10的周壁11和分隔壁12的壁部13一次性挤出成型来进行制作。
(密封工序)
密封工序是将密封材料糊填充在由成型工序得到的蜂窝成型体的孔道S的端部来形成密封部14的工序。作为密封材料糊，可以采用与上述的原料混合物同样的物质，但优选不包含有机纤维。通过不使用有机纤维，能够减小密封部14的气孔率。由密封工序形成了密封部14的蜂窝成型体根据需要进行干燥。需要说明的是，密封工序也可以在后述的脱脂工序或烧制工序之后进行。
(脱脂工序)
脱脂工序是将形成了密封部14的蜂窝成型体脱脂来形成脱脂体的工序，换言之，是将蜂窝成型体加热来除去蜂窝成型体中包含的有机成分的工序。脱脂工序中，长条状的有机纤维消失，由此能够在壁部13形成线状的气孔。脱脂工序可以使用公知的单独炉、所谓分批炉或连续炉来进行。脱脂温度没有特别限定，优选为300～800℃、更优选为400～750℃。脱脂时间没有特别限定，优选在上述的脱脂温度保持1～10小时，更优选保持2～5小时。脱脂气氛没有特别限定，优选氧浓度为0.1～20％。
(烧制工序)
烧制工序是对于由脱脂工序得到的脱脂体进行烧制来制作蜂窝过滤器10的工序。通过进行烧制，CZ复合氧化物等的颗粒间利用无机粘结剂进行结合，由此提高蜂窝过滤器10的机械强度。烧制工序可以使用公知的单独炉、所谓分批炉或连续炉来进行。烧制温度没有特别限定，优选为800～1300℃、更优选为900～1200℃。烧制时间没有特别限定，优选在上述的烧制温度保持1～20小时、更优选保持1～15小时。烧制气氛没有特别限定，优选氧浓度为1～20％。烧制工序可以使用与脱脂工序不同的炉另行进行，也可以使用与脱脂工序相同的炉连续进行。通过经历上述的混合工序、成型工序、密封工序、脱脂工序、烧制工序，可以制造出具有包含CZ复合氧化物的显示出上述特定的气孔径分布的壁部13的本实施方式的蜂窝过滤器10。
(负载工序)
负载工序是将催化剂负载于由烧制工序得到的蜂窝过滤器10的工序。作为催化剂的负载方法，例如可以举出将蜂窝过滤器10浸渍在包含催化剂的颗粒或络合物的溶液中，之后拉起蜂窝过滤器10并进行加热的方法。通过负载催化剂，蜂窝过滤器10的壁部13具备以CZ复合氧化物作为构成成分的基材、以及负载于该基材的催化剂。
对本实施方式的作用和效果进行说明。
(1)通过使蜂窝过滤器具备由以CZ复合氧化物和无机粘结剂作为构成成分的基材构成的壁部，与在由碳化硅等基材构成的壁部被覆有CZ复合氧化物的构成相比，在为相同的CZ复合氧化物的含量时能够减小壁部的热容量。另外，作为处理对象的气体通过在气孔径为0.01μm以上且小于1μm的范围具有峰的气孔而能够效率良好地扩散到壁部的内部。由此可提高扩散在壁部的内部的气体的净化性能。另外，通过存在有在气孔径为1μm以上50μm以下的范围具有峰的气孔，壁部的气体透过性提高，因此在具有作为捕集微粒的过滤器的功能的同时还能够将压力损失抑制得较低。
(2)壁部具有贯穿壁部的直径为1μm以上50μm以下的线状的气孔。因此，气体容易通过贯穿壁部的气孔而穿过壁部，由此可适当地提高壁部的气体透过性。
(3)壁部的基材包含氧化铝作为构成成分。因此，能够将所负载的催化剂高分散，由此能够提高作为处理对象的气体的净化性能。另外，能够提高高温状态下的壁部的机械强度。
(4)壁部的基材具备所负载的催化剂。因此，蜂窝过滤器不仅能够发挥出捕集微粒的功能，而且还能够发挥出作为处理对象的气体的净化作用等基于催化剂的功能。
(5)在催化剂为贵金属的情况下，由于二氧化铈-氧化锆复合氧化物具有作为促进由贵金属构成的催化剂的催化作用的助催化剂的功能，因此蜂窝过滤器能够发挥出高催化作用。
(6)蜂窝过滤器具有多个孔道，该多个孔道被壁部分隔、并且从上述蜂窝过滤器的作为一端侧的第1端部延伸至作为另一端侧的第2端部。孔道具备：第1端部侧的端部开放、第2端部侧的端部密封的第1孔道；与第1孔道相邻且第1端部侧的端部密封、第2端部侧的端部开放的第2孔道；以及与第1孔道和第2孔道中的至少一者相邻且第1端部侧的端部和第2端部侧的端部这两个端部开放的第3孔道。因此，能够利用第1孔道与第2孔道间的壁部捕集微粒。另外，通过具备第1端部侧的端部和第2端部侧的端部这两个端部开放的第3孔道，能够降低蜂窝过滤器的压力损失。
本实施方式还能够如下进行变更来实施。另外，也可以将上述实施方式的构成和以下的变更例中示出的构成适宜地组合来实施。
·本实施方式中，壁部由周壁和分隔壁构成，但也可以仅由分隔壁构成。这种情况下，可以通过在分隔壁的外周形成外周涂层来形成蜂窝过滤器。
·构成壁部的基材可以不必包含氧化铝作为构成成分。另外，在蜂窝过滤器的原料中也可以不必包含氧化铝颗粒。
·蜂窝过滤器可以不必具备第3孔道。即，全部孔道可以为将其两端部的任意一个密封的构成。利用该构成，能够提高蜂窝过滤器的捕集效率。
实施例
下面对进一步具体说明上述实施方式的实施例进行说明。
(实施例1)
将下述原料混合，制备原料混合物。
平均粒径为2μm的CZ复合氧化物颗粒：24.0质量％
平均粒径为2μm的θ-氧化铝颗粒：12.0质量％
平均纤维径为3μm、平均纤维长为60μm的α氧化铝纤维(无机纤维)：5.0质量％
平均纤维径为30μm、平均纤维长为1mm的丙烯腈系纤维(有机纤维)：13.0质量％
勃姆石(无机粘结剂)：10.0质量％
甲基纤维素(有机粘结剂)：7.0质量％
聚氧乙烯油基醚(成型助剂)：4.0质量％
离子交换水(分散介质)：25.0质量％
使用该原料混合物，利用挤出成型机成型出圆柱状的成型体。接着，将该成型体切断成规定的长度制作蜂窝成型体，之后如图2所示，将特定孔道的端部利用密封剂密封，形成密封部。密封剂的组成中，除了不包含有机纤维以外，与上述原料混合物为相同的组成。另外，密封部的长度为约3mm。接着，将蜂窝成型体干燥后，在700℃进行3小时脱脂，在1100℃烧制10小时，由此制作蜂窝过滤器。所得到的蜂窝过滤器是直径为117mm、长度为80mm的圆柱状，孔道的密度为46个/cm2(300cpsi)、壁部的厚度为0.254mm(10mil)。
接着，将二亚硝基二氨钯硝酸溶液([Pd(NH3)2(NO2)2]HNO3、钯浓度100g/L)和硝酸铑溶液([Rd(NO3)3]、铑浓度50g/L)以3：1的体积比例混合，制备混合溶液。将由上述工序制造的蜂窝过滤器浸渍在该混合溶液中，保持15分钟。之后在110℃干燥2小时，在氮气气氛中在500℃烧制1小时，由此使钯催化剂和铑催化剂负载于蜂窝过滤器。关于催化剂的负载量，以钯和铑的合计计，相对于蜂窝过滤器的单位表观体积为0.14g/L。
(比较例1)
在实施例1的原料中省略有机纤维，将除此以外的原料的混配比直接进行与实施例1相同的过程，由此制作出比较例1的蜂窝过滤器。
(比较例2)
首先将下述原料物混合，制备原料混合物。
平均粒径为15μm的碳化硅颗粒：28质量％
平均粒径为0.95μm的碳化硅颗粒：19质量％
平均粒径为34μm的白砂中空球(造孔剂)：9质量％
平均粒径为28μm的淀粉(造孔剂)：16质量％
甲基纤维素(有机粘结剂)：5质量％
山梨聚糖脂肪酸酯(分散剂)：3质量％
聚氧化烯系化合物(增塑剂)：2质量％
水(分散介质)：18质量％
使用该原料混合物，利用挤出成型机成型出棱柱状的成型体。接着，将该成型体切断，制作蜂窝成型体，之后使孔道相互交错地利用与上述原料混合物相同组成的封孔剂进行封孔。接着，将切断蜂窝成型体时的切去端(切れ端)用作支持材，在将蜂窝成型体载置在该支持材上的状态下，将蜂窝成型体在450℃加热5小时，由此得到去除了有机成分的脱脂体。进一步，在保持将脱脂体载置在支持材上的状态下，在氩气氛下在2000℃保持4.5小时，得到蜂窝烧制体。接着，将蜂窝烧制体在氮分压10kPa的氮气气氛下在800℃保持4.5小时，进行氮化工序，由此制作出纵34.4mm×横34.3mm×长80mm、孔道密度为46.5个/cm2(300cpsi)、壁部的厚度为0.254mm的以碳化硅作为主成分的蜂窝结构体。所得到的蜂窝结构体的平均气孔径为20μm、气孔率为60％。将该蜂窝结构体用无机粘接材粘接，实施外周加工，由此制作出直径为117mm、长度为80mm的圆柱状的蜂窝结构体。
接着，将使钯负载于γ-氧化铝颗粒而得到的颗粒与使铑负载于CZ复合氧化物而得到的颗粒以1：2混合，洗涂在上述圆柱状的蜂窝结构体上，制作蜂窝过滤器。关于此时催化剂的负载量，以钯和铑的合计计，相对于蜂窝过滤器的单位表观体积为0.14g/L。
(评价试验)
对于实施例和比较例的蜂窝过滤器，通过以下的方法测定气孔径分布、预热性能和压力损失。
(气孔径分布测定)
将实施例1和比较例1的蜂窝过滤器的壁部的气孔径分布的测定结果分别示于图3和图4。壁部的气孔径分布利用压汞法在接触角为130°、表面张力为485mN/m的条件下测定，使气孔径和log微分细孔容积分别表示为横轴和纵轴。
如图3所示，实施例1中，在气孔径为0.01μm以上且小于1μm的范围确认到1个峰，并且在气孔径为1μm以上50μm以下的范围确认到1个峰。与之相对，如图4所示，比较例1中，尽管在气孔径为0.01μm以上且小于1μm的范围能够确认到1个峰，但在气孔径为1μm以上50μm以下的范围未确认到峰。
(预热性能测定)
将以气密状态配置有实施例1和比较例1、2的各蜂窝过滤器的金属管与V型6汽缸3.5L发动机的排气管连接，测定从理论空燃比发动机启动到HC浓度((HC的流入量-HC的流出量)/(HC的流入量)×100)达到50％以下为止所需要的时间，对预热性能进行评价。
(压力损失测定)
使用图5所示的压力损失测定装置20对实施例1和比较例1、2的蜂窝过滤器的压力损失进行测定。图5是示意性示出压力损失测定方法的截面图。首先将蜂窝过滤器10以气密状态配置在金属管21中。连接于鼓风机22的金属管23与该金属管21连接。之后，使流速为10m/s的空气从鼓风机22向蜂窝过滤器10中流通，利用压力计24测定蜂窝过滤器10前后的压力差(压力损失)。
将预热性能测定和压力损失测定的结果列于表1。
[表1]
HC的净化率达到50％的时间(s) 压力损失(kPa)
实施例1 12 14.8
比较例1 20 52.9
比较例2 25 12.5
如表1所示，与比较例1、2的蜂窝过滤器相比，实施例1的蜂窝过滤器中，确认到烃(HC)的净化率达到50％为止的时间短、预热性能优异。另外，实施例1的蜂窝过滤器的压力损失低于比较例1的蜂窝过滤器，确认到其发挥出作为捕集微粒的过滤器的功能。
符号的说明
10…蜂窝过滤器、11…周壁、12…分隔壁、13…壁部、14…密封部、S…孔道。

Claims (7)

1.一种蜂窝过滤器，其是用于微粒的捕集的蜂窝过滤器，其中，
该蜂窝过滤器具备由基材构成的壁部，该基材以二氧化铈-氧化锆复合氧化物和无机粘结剂作为构成成分，
所述壁部在将由压汞法测定的气孔径和log微分细孔容积分别作为横轴和纵轴的气孔径分布中在气孔径为0.01μm以上且小于1μm的范围具有峰、并且在气孔径为1μm以上50μm以下的范围具有峰，所述壁部具有贯穿该壁部的直径为1μm以上50μm以下的线状的气孔，
蜂窝过滤器具有多个孔道，该多个孔道被所述壁部分隔、并且从所述蜂窝过滤器的作为一端侧的第1端部延伸至作为另一端侧的第2端部，
所述孔道具备：所述第1端部侧的端部开放、所述第2端部侧的端部密封的第1孔道；以及，与所述第1孔道相邻且所述第1端部侧的端部密封、所述第2端部侧的端部开放的第2孔道。
2.如权利要求1所述的蜂窝过滤器，其中，所述基材包含氧化铝作为构成成分。
3.如权利要求1或2所述的蜂窝过滤器，其中，催化剂被负载于所述基材。
4.如权利要求3所述的蜂窝过滤器，其中，所述催化剂为贵金属。
5.如权利要求1或2所述的蜂窝过滤器，其中，
所述孔道进一步具备：与所述第1孔道和所述第2孔道中的至少一者相邻且所述第1端部侧的端部和所述第2端部侧的端部这两个端部开放的第3孔道。
6.如权利要求3所述的蜂窝过滤器，其中，
所述孔道进一步具备：与所述第1孔道和所述第2孔道中的至少一者相邻且所述第1端部侧的端部和所述第2端部侧的端部这两个端部开放的第3孔道。
7.如权利要求4所述的蜂窝过滤器，其中，
所述孔道进一步具备：与所述第1孔道和所述第2孔道中的至少一者相邻且所述第1端部侧的端部和所述第2端部侧的端部这两个端部开放的第3孔道。
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