CN111747751A - 陶瓷多孔体及其制造方法、以及集尘用过滤器 - Google Patents
陶瓷多孔体及其制造方法、以及集尘用过滤器 Download PDFInfo
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- CN111747751A CN111747751A CN202010222314.1A CN202010222314A CN111747751A CN 111747751 A CN111747751 A CN 111747751A CN 202010222314 A CN202010222314 A CN 202010222314A CN 111747751 A CN111747751 A CN 111747751A
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Abstract
本发明提供一种陶瓷多孔体及其制造方法、以及集尘用过滤器,所述陶瓷多孔体的耐久性优异,并且,在用作集尘用过滤器的情况下,能够提高废气净化性能。陶瓷多孔体具备骨架部和细孔部,该骨架部包含骨料及粘结材料,该细孔部形成于骨架部之间,且能够供流体流通。该陶瓷多孔体的细孔部中,细孔径为10~15μm的细孔的细孔容积率为4~17%。
Description
技术领域
本发明涉及陶瓷多孔体及其制造方法、以及集尘用过滤器。
背景技术
从柴油发动机、汽油发动机等内燃机、各种燃烧装置等中排出的废气中包含大量的烟灰等粒子状物质(以下也称为“颗粒物”或“PM”)。如果该PM直接释放到大气中,则引起环境污染,因此,在废气的排气系统中搭载有用于捕集PM的集尘用过滤器(以下也称为“颗粒过滤器”)。作为集尘用过滤器,例如可以举出从柴油发动机、汽油发动机中排出的废气的净化用的柴油颗粒过滤器(DPF)、汽油颗粒过滤器(GPF)等。上述DPF及GPF使用具有通过隔壁而区划形成多个隔室的蜂窝结构的陶瓷多孔体,该多个隔室从第一端面贯通至第二端面,形成废气的流路。并且,要求该用途中使用的陶瓷多孔体具有提高PM的捕集率的细孔结构。
另外,上述集尘用过滤器所使用的陶瓷多孔体随着使用而在表面或内部堆积烟灰等粒子状物质。结果,陶瓷多孔体的压力损失增大,无法充分得到作为集尘用过滤器的捕集能力。因此,出于使作为集尘用过滤器的捕集能力再生的目的,进行使堆积于陶瓷多孔体的表面或内部的粒子状物质定期燃烧而除去的再生处理。从稳定地进行该再生处理的观点出发,还要求陶瓷多孔体具有针对再生处理的耐久性。
另外,上述废气中还包含NOx、CO及HC等有害物质。在减少废气中的有害物质的量并净化废气时,广泛使用催化反应。在上述利用了催化反应的废气净化中,作为用于担载SCR催化剂等废气净化催化剂的载体,也使用上述具有蜂窝结构的陶瓷多孔体。并且,从提高废气净化性能的观点出发,要求该用途中使用的陶瓷多孔体具有能够担载大量废气净化催化剂的细孔结构。
作为如上所述的用途中使用的现有的陶瓷多孔体,例如专利文献1中提出了如下陶瓷多孔体,其中,中值细孔径(d50)为10μm以上,(中值细孔径(d50)-中值细孔径(d10))/中值细孔径(d50)的值小于0.8,总气孔率中少于5%由细孔径小于1.0μm的细孔形成。
另外,专利文献2中提出如下陶瓷多孔体,其中,每单位体积的、细孔径为15μm以下的细孔容积及细孔径为40μm以上的细孔容积分别为0.7cc/cc以下。
现有技术文献
专利文献
专利文献1:日本特许第5897242号公报
专利文献2:日本特许第4954705号公报
发明内容
然而,专利文献1及2中记载的陶瓷多孔体虽然着眼于细孔结构,但是不能说它们的细孔结构是最佳的。因此,在将该陶瓷多孔体作为集尘用过滤器进行使用的情况下,存在废气净化性能并不充分的问题。应予说明,本说明书中“废气净化性能”的含义包括:PM的捕集性能及NOx等有害物质的净化性能。
本发明是为了解决如上所述的问题而实施的,其目的在于,提供耐久性优异、且在用作集尘用过滤器的情况下能够提高废气净化性能的陶瓷多孔体及其制造方法。
另外,本发明的目的在于,提供耐久性优异、且废气净化性能高的集尘用过滤器。
本发明的发明人为了解决如上所述的问题进行了潜心研究,结果注意到:陶瓷多孔体的细孔径为10~15μm的细孔容积率与耐久性及废气净化性能密切相关,并发现:将陶瓷多孔体的细孔径为10~15μm的细孔容积率控制在特定的范围内,由此能够使耐久性及废气净化性能得到提高,以至完成本发明。
即,本发明是一种陶瓷多孔体,其具备骨架部和细孔部,该骨架部包含骨料及粘结材料,该细孔部形成于所述骨架部之间,且能够供流体流通,所述细孔部中,细孔径为10~15μm的细孔的细孔容积率为4~17%。
另外,本发明是一种陶瓷多孔体的制造方法,其包括以下工序:将包含骨料、粘结材料、烧成助剂、造孔剂及粘合剂的坯土成型而得到成型体的工序、以及对所述成型体进行烧成的工序,
所述骨料的体积基准下的累积粒度分布中,50%粒径D50为15~30μm,且(90%粒径D90-10%粒径D10)/50%粒径D50为1.0以下,
所述烧成助剂的配合量相对于所述骨料及所述粘结材料的合计100质量份而言为1.0~4.0质量份。
此外,本发明是具有所述陶瓷多孔体的集尘用过滤器。
发明效果
根据本发明,能够提供耐久性优异、且在用作集尘用过滤器的情况下能够提高废气净化性能的陶瓷多孔体及其制造方法。
另外,根据本发明,能够提供耐久性优异、且废气净化性能高的集尘用过滤器。
附图说明
图1是实施方式1的陶瓷多孔体的SEM照片。
图2是示意性地表示实施方式2的陶瓷多孔体的立体图。
图3是示意性地表示实施方式2的陶瓷多孔体的与隔室延伸的方向平行的截面的截面图。
图4是应用了实施方式2的陶瓷多孔体的蜂窝催化器中的、将与隔室延伸的方向正交的截面的一部分放大的局部放大截面图。
符号说明
1…隔壁、2…隔室、2a…流入隔室、2b…流出隔室、8…封孔部、11…第一端面、12…第二端面、15…接合层、17…蜂窝单元、20…外周涂层、22…催化剂、100…蜂窝结构体。
具体实施方式
以下,对本发明的陶瓷多孔体及其制造方法、以及集尘用过滤器的优选实施方式具体地进行说明,但是,本发明并不限定于此进行解释,只要不脱离本发明的主旨,就可以基于本领域技术人员的知识进行各种变更、改良等。各实施方式中公开的多个构成要素可以通过适当的组合而形成各种发明。例如,可以从实施方式中所示的全部构成要素中删除若干构成要素,也可以将不同实施方式的构成要素进行适当组合。
(实施方式1)
图1是本实施方式的陶瓷多孔体的SEM照片。
如图1所示,本实施方式的陶瓷多孔体具备骨架部和细孔部,该骨架部包含骨料及粘结材料,该细孔部形成于骨架部之间,且能够供流体流通。
此处,细孔部的细孔径及细孔容积率与陶瓷多孔体的耐久性、废气净化性能等各种特性相关联,如果提高细孔径较小的细孔的细孔容积率,则耐久性提高,但存在NOx等有害物质的净化性能降低的趋势。特别是,以往认为,在细孔径为15μm以下的较小的细孔中,废气不易流动,对提高有害物质的净化性能而言几乎没有帮助,因此,希望细孔径为15μm以下的较小的细孔的细孔容积率较低。
然而,根据本发明的发明人的研究结果可知:细孔径为10~15μm的细孔对有害物质净化性能的影响较大,控制其细孔容积率对于提高有害物质的净化性能是有效的。
因此,本实施方式的陶瓷多孔体中,将细孔径为10~15μm的细孔的细孔容积率控制在4~17%。通过使该细孔容积率在上述的范围内,能够同时提高有害物质的净化性能及耐久性。另外,从稳定地得到上述效果的观点出发,该细孔容积率优选为5~13%。
此处,本说明书中“细孔径”是指:依据JIS R1655:2003并通过水银压入法求出的细孔分布中的细孔径。
另外,细孔径小于10μm的细孔对于提高有害物质的净化性能几乎没有帮助,因此,希望细孔径小于10μm的细孔较少。因此,细孔径小于10μm的细孔的细孔容积率优选为9.5%以下,更优选为7%以下。通过使该细孔容积率为上述的范围,能够使有害物质的净化性能得到提高。
另外,细孔径超过40μm的细孔有可能导致耐久性及PM的捕集性能降低,因此,希望细孔径超过40μm的细孔较少。因此,细孔径超过40μm的细孔的细孔容积率优选为17%以下,更优选为14%以下。通过使该细孔容积率为上述的范围,能够同时提高耐久性及PM的捕集性能。
作为骨架部中使用的骨料,没有特别限定,可以使用该技术领域中公知的骨料。其中,骨料优选为碳化硅、氮化硅、氮化铝、多铝红柱石、氧化钛或包含氧化钛的复合氧化物(例如钛酸铝)。通过将上述材料用作骨料,能够得到强度及耐热冲击性优异的陶瓷多孔体。
骨料的平均粒径优选为40μm以下,更优选为30μm以下。通过使用具有上述范围的平均粒径的骨料,不易形成粗大的骨架部,容易在骨架部之间形成连通性良好的细孔部。另外,骨料的平均粒径的下限没有特别限定,优选为10μm,更优选为15μm。
此处,本说明书中“平均粒径”是指:利用激光衍射散射法求出的累积粒度分布(体积基准)中的积算值50%处的粒径。
作为骨架部中使用的粘结材料,没有特别限定,可以使用该技术领域中公知的粘结材料。其中,粘结材料优选为选自由金属硅、碳化硅、氧化铝及包含氧化铝的复合氧化物(例如堇青石)构成的组中的至少1种。通过按适当选择相对于骨料的比率的方式使用上述粘结材料,能够得到热传导性优异的陶瓷多孔体。
应予说明,碳化硅也可以作为骨料进行使用,不过,根据一同使用的骨料的种类、烧成温度,还作为粘结材料发挥作用。例如,使用作为骨料的碳化硅、以及包含Si及C的有机物作为原料的情况下,该有机物于约1800℃反应烧结而生成的碳化硅作为粘结材料发挥作用。
骨架部可以进一步包含源自于烧成助剂的氧化物。此处,源自于烧成助剂的氧化物的种类可以根据使用的烧成助剂的种类及烧成温度来确定。
作为烧成助剂,没有特别限定,可以使用该技术领域中公知的烧结助剂。烧成助剂通常含有包含碱土金属元素的化合物。作为包含碱土金属的化合物的例子,可以举出钙、镁或锶的氟化物、碳化物、氯化物、硅化物、碳酸盐、氢氧化物、氧化物、无机酸盐、有机酸盐等。它们可以单独使用,或者2种以上组合使用。另外,从控制烧成助剂的熔点的观点出发,烧成助剂可以进一步含有包含碱土金属元素以外的元素的化合物。
烧成助剂优选为包含含有锶的化合物和含有铝的化合物的混合物。此处,各化合物可以含有2种以上金属元素。例如,烧成助剂为包含氧化锶及氧化铝的混合物或在烧成时提供该混合物的原料。作为在烧成时提供氧化锶的原料,可以举出碳酸锶。作为在烧成时提供氧化铝的原料,可以举出氢氧化铝。
陶瓷多孔体的气孔率没有特别限定,优选为55%以上,更优选为60%以上。通过采用上述范围的气孔率,能够确保废气的流动容易度,使废气净化性能得到提高。另一方面,气孔率的上限没有特别限定,优选为68%,更优选为65%。通过使气孔率的上限为上述的值,能够确保耐久性。
此处,本说明书中“气孔率”是指:依据JIS R1655:2003并通过水银压入法测定得到的气孔率。
具有上述特征的陶瓷多孔体可以通过如下方法来制造,该方法包括:将包含骨料、粘结材料、烧成助剂、造孔剂及粘合剂的坯土成型而得到成型体的工序、以及对成型体进行烧成的工序。
该方法中,骨料的体积基准下的累积粒度分布中,50%粒径D50为15~30μm,优选为16~28μm,更优选为18~26μm。另外,骨料的体积基准下的累积粒度分布中,(90%粒径D90-10%粒径D10)/50%粒径D50为1.0以下,优选为0.8以下。通过使用具有上述粒度分布的骨料作为原料,能够减少对于提高有害物质的净化性能几乎没有帮助的细孔径小于10μm的细孔及有可能导致耐久性、PM的捕集性能降低的细孔径超过40μm的细孔,因此,能够得到具有所期望的细孔结构的陶瓷多孔体。
此处,本说明书中,50%粒径D50是指:利用激光衍射散射法求出的累积粒度分布(体积基准)中的积算值50%处的粒径。同样地,90%粒径D90及10%粒径D10分别是指:利用激光衍射散射法求出的累积粒度分布(体积基准)中的积算值90%及10%处的粒径。
骨料的90%粒径D90没有特别限定,优选为10~45μm,更优选为20~40μm。另外,骨料的10%粒径D10没有特别限定,优选为5~20μm,更优选为10~18μm。通过使用具有上述粒度分布的骨料作为原料,能够稳定地得到上述效果。
骨料及粘结材料的配合量根据种类进行适当设定即可,没有特别限定,骨料与粘结材料的质量比例优选为70:30~85:15。通过使该配合量为上述范围,容易得到具有所期望的细孔结构的陶瓷多孔体。
烧结助剂具有提高骨料和粘结材料的浸润性的作用。因此,如果烧结助剂的含量较多,则在烧成时,骨料与粘结材料的接触面积增大,所以,耐久性(强度)提高,但不易得到所期望的细孔结构。
因此,从提高耐久性且得到所期望的细孔结构的观点出发,烧结助剂的配合比例相对于骨料及粘结材料的合计100质量份而言为1.0~4.0质量份,优选为1.8~3.2质量份。
造孔剂是出于调整陶瓷多孔体的气孔率及细孔径的目的而配合的。作为造孔剂,没有特别限定,可以使用该技术领域中公知的造孔剂。作为造孔剂的例子,可以举出石墨、小麦粉、交联淀粉、发泡树脂、酚醛树脂、聚甲基丙烯酸甲酯、聚乙烯、聚对苯二甲酸乙二醇酯等。它们可以单独使用,或者可以2种以上组合使用。
造孔剂的50%粒径D50没有特别限定,优选为25~45μm,更优选为30~40μm。另外,造孔剂的(90%粒径D90-10%粒径D10)/50%粒径D50没有特别限定,优选为1.2以下,更优选为1.0以下。通过使用具有上述粒度分布的造孔剂作为原料,容易得到具有所期望的细孔径及气孔率的陶瓷多孔体。
造孔剂的90%粒径D90没有特别限定,优选为10~60μm,更优选为20~50μm。另外,造孔剂的10%粒径D10没有特别限定,优选为5~23μm,更优选为10~22μm。通过使用具有上述粒度分布的造孔剂作为原料,能够稳定地得到上述效果。
坯土中的造孔剂的配合比例根据种类进行适当设定即可,没有特别限定,相对于骨料及粘结材料的合计100质量份而言,优选为5~35质量份,更优选为10~30质量份,进一步优选为15~25质量份。
作为粘合剂,没有特别限定,可以使用该技术领域中公知的粘合剂。作为粘合剂的例子,可以举出甲基纤维素、羟丙基甲基纤维素等有机粘合剂、蒙脱石、海泡石等无机粘合剂。它们可以单独使用,或者可以2种以上组合使用。
坯土中的粘合剂的配合量根据种类进行适当设定即可,没有特别限定,相对于骨料及粘结材料的合计100质量份而言,优选为3~17质量份,更优选为5~15质量份,进一步优选为7~13质量份。
通过将上述的原料进行混合及混炼,能够得到坯土。作为原料的混合及混炼方法,没有特别限定,可以通过该技术领域中公知的方法来进行。例如,可以使用捏合机、真空练泥机等,进行原料的混合及混炼。
坯土的成型方法也同样地没有特别限定,可以通过该技术领域中公知的方法、例如挤出成型来进行。
成型体在烧成之前可以进行预烧,以便将成型体中包含的有机粘合剂除去(脱脂)。预烧优选在比金属硅熔融的温度更低的温度下进行。具体而言,可以在150~700℃左右的规定温度下暂时保持,另外,可以在规定温度区域内使升温速度降至50℃/小时以下进行预烧。
关于在规定的温度下暂时保持的方法,根据所使用的有机粘合剂的种类及量,可以仅在一个温度水平进行保持,也可以在多个温度水平进行保持,此外,在多个温度水平进行保持的情况下,可以使保持时间彼此相同,也可以不同。另外,关于减慢升温速度的方法,也同样地,可以仅在某一个温度区域间进行减慢,也可以在多个区间进行减慢,此外,在多个区间的情况下,可以使速度彼此相同,也可以不同。
关于预烧的气氛,可以为氧化气氛,不过,在成型体中包含大量有机粘合剂的情况下,预烧中,有机粘合剂有时因氧而剧烈燃烧,导致成型体温度急剧升高,因此,也可以通过在N2、Ar等不活泼性气氛中进行预烧来抑制成型体的异常升温。该异常升温的抑制是在使用了热膨胀系数较大的(不耐热冲击的)原料的情况下较为重要的控制。另外,除了骨料为碳化硅粒子的情况以外,在有可能于高温发生氧化的情况下,也优选至少在氧化开始的温度以上通过在如上所述的不活泼性气氛中进行预烧来抑制成型体的氧化。
预烧及后续的烧成可以在同一炉或者分开的炉中作为分开的工序来进行,或者可以为同一炉中的连续工序。在不同的气氛中实施预烧及烧成的情况下,前者是优选的方法,不过,从总烧成时间、炉的运转成本等角度考虑,也优选后者的方法。
关于烧成气氛,根据骨料的种类来确定即可。例如,在使用了有可能于高温发生氧化的骨料的情况下,优选至少在氧化开始的温度以上的温度区域采用N2、Ar等非氧化气氛。
如上所述制造的本实施方式的陶瓷多孔体中,细孔径为10~15μm的细孔容积率被控制在适当的范围内,因此,能够提高耐久性及废气净化性能。
(实施方式2)
本实施方式的陶瓷多孔体具有通过隔壁而区划形成多个隔室的蜂窝结构,该多个隔室从第一端面贯通至第二端面,形成流体的流路。上述具有蜂窝结构的陶瓷多孔体中,隔壁相当于陶瓷多孔体。另外,在具有蜂窝结构的陶瓷多孔体中,“与流体的流通方向平行的方向”是指与隔室延伸的方向正交的方向,“流体的流通方向”是指隔壁的厚度方向。
本实施方式的陶瓷多孔体除了具有规定的蜂窝结构以外,与实施方式1的陶瓷多孔体相同。因此,此处,对于与实施方式1共通的构成省略说明,仅对与实施方式1不同的部位进行说明。
图2是示意性地表示本实施方式的陶瓷多孔体的立体图。另外,图3是示意性地表示本实施方式的陶瓷多孔体的与隔室延伸的方向平行的截面的截面图。
如图2及图3所示,本实施方式的陶瓷多孔体(以下称为“蜂窝结构体100”)具备:多个柱状的蜂窝单元17、以及配置于这些多个蜂窝单元17的侧面间的接合层15。通过采用像这样的单元结构,能够使在将蜂窝结构体100作为集尘用过滤器进行使用时、蜂窝结构体100受到的应力得到缓和。
柱状的蜂窝单元17具备区划形成多个隔室2的隔壁1,该多个隔室2从第一端面11贯通至第二端面12,形成流体的流路。
作为隔壁1的厚度,没有特别限定,优选为100~500μm,更优选为150~450μm,进一步优选为125~400μm。通过使隔壁1的厚度为100μm以上,可充分确保隔壁1的强度,在将蜂窝结构体100收纳于罐体时,蜂窝结构体100不易破损。另外,通过使隔壁1的厚度为500μm以下,能够抑制压力损失增大。
作为蜂窝单元17中的隔室密度,没有特别限定,优选为15~100隔室/cm2,更优选为30~65隔室/cm2,进一步优选为30~50隔室/cm2。通过使隔室密度为15隔室/cm2以上,可充分确保隔壁1的强度,在将蜂窝结构体100收纳于罐体时,蜂窝结构体100不易破损。通过使隔室密度为100隔室/cm2以下,能够抑制压力损失增大。
作为隔室2的形状,没有特别限定,可以为该技术领域中公知的形状。此处,本说明书中“隔室2的形状”是指:与隔室2延伸的方向正交的方向的截面中的隔室2的形状。作为隔室2的形状的例子,可以举出圆形、四边形、六边形、八边形等。特别是,四边形中,优选为正方形或长方形。
作为蜂窝结构体100的形状,没有特别限定,可以为端面(第一端面11及第二端面12)为圆形的柱状(圆柱形状)、端面为椭圆形状的柱状、端面为多边形(例如四边形、五边形、六边形、七边形、八边形等)的柱状等。
蜂窝结构体100的第一端面11至第二端面12为止的长度及与隔室2延伸的方向正交的截面的大小根据蜂窝结构体100的使用状况及使用用途等进行适当设定即可,没有特别限定。
如图2及图3所示,蜂窝结构体100可以具备封孔部8,该封孔部8设置于第一端面11中的规定隔室2(流出隔室2b)的开口部及第二端面12中的剩余隔室2(流入隔室2a)的开口部。在将蜂窝结构体100用于DPF等的情况下,优选为上述结构。即,通过具备封孔部8,使得流入至蜂窝结构体100的废气由隔壁1进行过滤,因此,能够良好地捕集废气中的粒子状物质。应予说明,蜂窝结构体100中,流入隔室2a和流出隔室2b交替排列。由此,在蜂窝结构体100的第一端面11及第二端面12分别呈现出由封孔部8和隔室2的开口部形成的棋盘格状。
封孔部8的材质和蜂窝单元17的材质可以为相同的材质,也可以为不同的材质。
蜂窝结构体100可以在其外周面具有外周涂层20。该外周涂层20可以采用与蜂窝单元17相同的材质。通过形成外周涂层20,即便在蜂窝结构体100的输送中等受到外力,也不易产生缺口等缺陷。
对于蜂窝结构体100,通过将催化剂担载于隔壁1,能够用作对废气中包含的一氧化碳等被净化成分进行净化的蜂窝催化器。例如,如图4所示,可以使催化剂22按将区划形成隔室2的隔壁1的气孔填埋的方式进行附着。应予说明,图4是将应用了本实施方式的陶瓷多孔体的蜂窝催化器中的、与隔室延伸的方向正交的截面的一部分放大的局部放大截面图。另外,图4中,催化剂22呈点状分布,不过,催化剂22的分布状态没有特别限定。
作为催化剂22,可以使用该技术领域中公知的催化剂。作为催化剂22的例子,可以举出汽油发动机废气净化三元催化剂、汽油发动机或柴油发动机废气净化用的氧化催化剂、NOx选择性还原用的SCR催化剂等。具体而言,可以使用包含铂、钯、铑、铱、银等贵金属、氧化铝、氧化锆、二氧化钛、氧化铈、氧化铁等氧化物、铜离子交换沸石的单体或化合物等。这些催化剂可以单独使用,或者可以2种以上组合使用。
作为具有上述特征的蜂窝结构体100的制造方法,没有特别限定,可以基于该技术领域中公知的方法来进行。具体而言,可以如下进行。
首先,将坯土挤出成型为具有蜂窝结构的柱状成型体(与蜂窝单元17的形状相对应的成型体),除此以外,与实施方式1同样地制作蜂窝单元17。可以使用具有所期望的隔室形状、隔壁厚度、隔室密度的口模来进行挤出成型。这样得到的柱状成型体可以在烧成前使其干燥。作为干燥方法,没有特别限定,可以使用热风干燥、微波干燥、介电干燥、减压干燥、真空干燥、冷冻干燥等。其中,优选将介电干燥、微波干燥或热风干燥单独或组合进行。另外,作为干燥条件,没有特别限定,优选采用干燥温度30~150℃、干燥时间1分钟~2小时。本说明书中“干燥温度”是指:进行干燥的气氛的温度。
接下来,将上述得到的柱状成型体或其干燥体封孔。作为将隔室2的开口部封孔的方法,使用向隔室2的开口部填充封孔材料的方法即可。作为填充封孔材料的方法,可以依据以往公知的具备封孔部8的蜂窝结构体100的制造方法来进行。封孔用的封孔部形成原料可以使用以往公知的蜂窝结构体100的制造方法中使用的封孔部形成原料。
接下来,对进行了封孔的柱状成型体或其干燥体进行预烧,将有机粘合剂除去(脱脂)后,进行正式烧成,由此得到蜂窝单元17。得到的蜂窝单元17进一步在含氧气氛中实施热处理,由此,可以在表面形成氧化被膜。
接下来,在上述得到的蜂窝单元17的侧面涂布接合材料,按蜂窝单元17的侧面彼此对置的方式相邻配置。然后,将相邻的蜂窝单元17彼此压接后,进行加热干燥,由此得到蜂窝结构体100。此时,接合材料因加热干燥而成为接合层15。
作为接合材料,没有特别限定,例如可以使用将陶瓷粉末、分散介质(例如水等)以及根据需要所添加的粘合剂、胶溶剂、发泡树脂等添加剂混合而制备的接合材料。作为陶瓷,没有特别限定,优选为含有选自由堇青石、多铝红柱石、锆石、钛酸铝、碳化硅、氮化硅、氧化锆、尖晶石、印度石、假蓝宝石、刚玉及二氧化钛构成的组中的至少1种的陶瓷,更优选为与蜂窝单元17相同的材质。作为粘合剂,可以使用聚乙烯醇、甲基纤维素、CMC(羧甲基纤维素)等。
接下来,对于如上所述得到的蜂窝结构体100,可以根据需要对外周部进行磨削加工,使其成为所期望的形状(例如圆柱状),在外周面涂布外周涂层材料后,进行加热干燥,形成外周壁。
实施例
以下,通过实施例,对本发明进一步具体地进行说明,本发明并不受这些实施例的任何限定。
(实施例1)
将具有表1所示的粒度分布的碳化硅(骨料)、金属硅(粘结材料)、具有表1所示的粒度分布的交联淀粉(造孔剂)、碳酸锶(烧成助剂)、氢氧化铝(烧成助剂)、粘合剂(羟丙基甲基纤维素(以下简称为“HPMC”)及蒙脱石)按表1所示的比例进行配合,加入水进行混合后,利用捏合机进行混炼,接下来,利用真空练泥机进行练泥,得到坯土。将得到的坯土利用挤出成型机成型为端面的一边长度为36mm、隔壁的厚度为300μm、隔室密度为46隔室/cm2的四棱柱状的蜂窝形状。接下来,对得到的成型体进行微波干燥后,于120℃进行热风干燥,得到干燥体。接下来,针对得到的蜂窝干燥体,在规定的隔室的一个端部和剩余隔室的另一个端部形成封孔部。应予说明,按规定隔室和剩余隔室交替(Alternately)排列的方式在两个端面通过隔室的开口部和封孔部而形成棋盘格状。封孔用的填充材料使用与蜂窝成型体同样的材料。接下来,将得到的封孔蜂窝干燥体在大气中、于450℃进行5小时脱脂后,将已脱脂的干燥体在Ar气氛中、于1430℃进行2小时烧成,得到蜂窝单元。
接下来,在蜂窝单元的侧面涂布接合材料,与其他蜂窝单元的侧面接合。反复进行该工序,制作将纵4个×横4个蜂窝单元接合得到的合计16个蜂窝单元层叠体。接下来,通过从外部施加压力而使蜂窝单元彼此压接后,于140℃进行2小时干燥,得到接合体。接下来,对接合体的外周进行切削加工,以使得到的接合体的与隔室延伸的方向正交的截面为圆形。接下来,在其加工面涂布与接合材料相同组成的外周涂层材料,然后,于700℃进行2小时干燥,形成外周涂层,得到蜂窝结构体。
(实施例2~6及比较例1~3)
像表1所示那样变更使用的原料及配合比例,除此以外,以与实施例1同样的条件得到蜂窝结构体。应予说明,实施例5中,作为粘合剂,使用HPMC及海泡石。
表1
对上述的实施例及比较例中得到的蜂窝结构体进行以下的评价。
(细孔容积率及气孔率)
使用压汞仪(Micromeritics公司制AutoporeIV9500),测定具有各细孔径的细孔的细孔容积。例如,通过细孔径为15μm的积算细孔容积的值减去细孔径为10μm的积算细孔容积的值,求出细孔径为10~15μm的细孔的细孔容积(mL/g)。另外,以细孔径为10~15μm的细孔的细孔容积相对于全部细孔容积的百分率的形式计算出细孔径为10~15μm的细孔的细孔容积率。应予说明,全部细孔容积(mL/g)是指每1g蜂窝结构体中的全部细孔的容积。另外,还与上述同样地求出具有其他细孔径的细孔的细孔容积及细孔容积率。
使用全部细孔容积(mL/g)及蜂窝结构体的真密度(g/mL),通过下式计算出气孔率。
气孔率=全部细孔容积/(全部细孔容积+1/蜂窝结构体的真密度)×100
(NOx净化率)
使NOx选择性还原用的SCR催化剂(铜离子交换沸石催化剂)100g/L担载于蜂窝结构体的隔壁。具体而言,使蜂窝结构体从一个端面浸渍于收纳有所述SCR催化剂的浆料的容器中,并从另一个端面吸引浆料,由此使SCR催化剂担载于隔壁。使包含NOx的试验用气体流通于该蜂窝结构体,利用气体分析仪,对从该蜂窝结构体中排出的气体的NOx量进行分析,求出NOx净化率。
此时,流入于蜂窝结构体的试验用气体的温度为200℃。应予说明,通过加热器来调节试验用气体的温度。加热器使用红外成像炉(Infrared image furnace)。试验用气体使用在氮中混合二氧化碳5体积%、氧14体积%、一氧化氮350ppm(体积基准)、氨350ppm(体积基准)及水10体积%得到的气体。关于该试验用气体,分别准备出水和将其他气体混合得到的混合气体,在进行试验时,使水和混合气体在配管中混合进行使用。气体分析仪使用“HORIBA公司制、MEXA9100EGR”。另外,试验用气体向陶瓷多孔体流入时的空间速度为100,000(小时-1)。“NOx净化率”是:试验用气体的NOx量减去从陶瓷多孔体中排出的气体的NOx量得到的值除以试验用气体的NOx量,乘以100得到的值(单位:%)。
应予说明,该评价中,将NOx净化率超过70%的情形表示为◎,将NOx净化率超过60%且为70%以下的情形表示为〇,将NOx净化率超过50%且为60%以下的情形评价为△,将NOx净化率为50%以下的情形表示为×。另外,NOx净化率如果超过50%(评价结果为△、〇及◎),则实用上没有问题,因此,评价为合格。
(PM捕集率)
将以与NOx净化率的评价相同的方法担载有SCR催化剂的蜂窝结构体安装于搭载有排气量2.0升的柴油发动机的乘用汽车的废气排气管。使用该乘用汽车,以EUDC(ExtraUrban Driving Cycle)模式行驶3次后,放置(Soak:发动机停止)8小时以上,然后,以NEDC(New European Driving Cycle)模式进行行驶。基于以该NEDC模式行驶时的、担载有SCR催化剂的蜂窝结构体的废气出口(流出侧)处的粒子状物质(PM)的个数累计和废气中的全部PM个数,通过下式,计算出PM捕集率。
PM捕集率[%]=(废气中的全部PM个数-蜂窝结构体的废气出口(流出侧)处的PM的个数累计)/废气中的全部PM个数×100
按照欧洲经济委员会的世界汽车标准协调论坛的废气能量专家会议通过粒子测定程序(简称为“PMP”)提出的方法,进行PM个数的测定。
应予说明,该评价中,将PM捕集率超过95%的情形表示为◎,将PM捕集率超过90%且为95%以下的情形表示为〇,将PM捕集率超过80%且为90%以下的情形表示为△,将PM捕集率为80%以下的情形表示为×。另外,PM捕集率如果超过80%(评价结果为△、〇及◎),则能够满足欧洲EURO6限制值6.0×1011个/km,实用上没有问题,因此,评价为合格。
(等静压强度)
基于社团法人汽车技术会发行的汽车标准(JASO标准)M505-87中规定的等静压破坏强度试验,进行等静压强度的测定。等静压破坏强度试验是:在橡胶筒状容器中放入蜂窝结构体并用铝制板盖上、在水中进行各向同性加压压缩的试验。即,等静压破坏强度试验是:模拟在罐体中蜂窝结构体的外周面被把持时的压缩负荷加重的试验。通过该等静压破坏强度试验测定的等静压强度用蜂窝结构体发生破坏时的加压压力值(MPa)表示。
应予说明,该评价中,将等静压强度超过2.0MPa的情形表示为◎,将等静压强度超过1.5MPa且为2.0MPa以下的情形表示为〇,将等静压强度超过1.0MPa且为1.5MPa以下的情形表示为△,将等静压强度为1.0MPa以下的情形表示为×。另外,等静压强度如果超过1.0MPa(评价结果为△、〇及◎),则实用上没有问题,因此,评价为合格。
(开裂临界温度)
通过使由燃烧器加热后的空气流通于蜂窝结构体,使得中心部分与外侧部分之间产生温度差,利用对蜂窝结构体的耐热冲击性进行评价的快速加热试验(燃烧器剥落试验)求出开裂临界温度(蜂窝结构体没有发生开裂的最高温度)。以试验温度(加热后的空气的温度)为900℃、1000℃、1100℃的顺序进行。然后,观察试验后的蜂窝结构体的开裂的发生状况。评价基准如下:将即便试验温度为1100℃也没有发生开裂的情形评价为◎,将虽然在试验温度1000℃没有发生开裂、但在试验温度1100℃发生了开裂的情形评价为〇,将虽然在试验温度900℃没有发生开裂、但在试验温度1000℃发生了开裂的情形评价为△,将在试验温度900℃发生了开裂的情形评价为×。另外,开裂临界温度如果为900℃以上(评价结果为△、〇及◎),则实用上没有问题,因此,评价为合格。
将上述的各评价结果示于表2。
表2
如表2所示,细孔径为10~15μm的细孔的细孔容积率在4~17%的范围内的实施例1~6的蜂窝结构体能够达成所有评价项目的合格基准。与此相对,细孔径为10~15μm的细孔的细孔容积率在4~17%的范围外的比较例1~3的蜂窝结构体无法达成任一评价项目的合格基准。
由以上结果可知,根据本发明,能够提供耐久性优异、且在作为集尘用过滤器使用的情况下能够提高废气净化性能的陶瓷多孔体及其制造方法。另外,根据本发明,能够提供耐久性优异、且废气净化性能高的集尘用过滤器。
Claims (12)
1.一种陶瓷多孔体,其特征在于,具备:
骨架部,该骨架部包含骨料及粘结材料;以及
细孔部,该细孔部形成于所述骨架部之间,且能够供流体流通,
所述细孔部中,细孔径为10~15μm的细孔的细孔容积率为4~17%。
2.根据权利要求1所述的陶瓷多孔体,其特征在于,
所述陶瓷多孔体的气孔率为55%以上。
3.根据权利要求1或2所述的陶瓷多孔体,其特征在于,
所述细孔部中,细孔径小于10μm的细孔的细孔容积率为9.5%以下。
4.根据权利要求1~3中的任一项所述的陶瓷多孔体,其特征在于,
所述细孔部中,细孔径超过40μm的细孔的细孔容积率为17%以下。
5.根据权利要求1~4中的任一项所述的陶瓷多孔体,其特征在于,
所述骨料为碳化硅、氧化钛或它们的混合物。
6.根据权利要求1~5中的任一项所述的陶瓷多孔体,其特征在于,
所述粘结材料为选自由金属硅、氧化铝及堇青石构成的组中的至少1种。
7.根据权利要求1~6中的任一项所述的陶瓷多孔体,其特征在于,
在所述细孔部内担载有催化剂。
8.根据权利要求1~7中的任一项所述的陶瓷多孔体,其特征在于,
所述陶瓷多孔体具有通过隔壁而区划形成有多个隔室的蜂窝结构,该多个隔室从第一端面贯通至第二端面,形成所述流体的流路。
9.根据权利要求8所述的陶瓷多孔体,其特征在于,
所述蜂窝结构包括封孔部,该封孔部设置于所述第一端面中的规定的所述隔室的开口部及所述第二端面中的剩余的所述隔室的开口部。
10.一种陶瓷多孔体的制造方法,其特征在于,包括以下工序:
将包含骨料、粘结材料、烧成助剂、造孔剂及粘合剂的坯土成型而得到成型体的工序、以及
对所述成型体进行烧成的工序,
所述骨料的体积基准下的累积粒度分布中,50%粒径D50为15~30μm,且(90%粒径D90-10%粒径D10)/50%粒径D50为1.0以下,
所述烧成助剂的配合量相对于所述骨料及所述粘结材料的合计100质量份而言为1.0~4.0质量份。
11.根据权利要求10所述的陶瓷多孔体的制造方法,其特征在于,
所述造孔剂的体积基准下的累积粒度分布中,50%粒径D50为25~45μm,且(90%粒径D90-10%粒径D10)/50%粒径D50为1.2以下。
12.一种集尘用过滤器,其特征在于,
具有权利要求1~9中的任一项所述的陶瓷多孔体。
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