CN110894157A - 蜂窝结构体的制造方法 - Google Patents
蜂窝结构体的制造方法 Download PDFInfo
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- CN110894157A CN110894157A CN201910853553.4A CN201910853553A CN110894157A CN 110894157 A CN110894157 A CN 110894157A CN 201910853553 A CN201910853553 A CN 201910853553A CN 110894157 A CN110894157 A CN 110894157A
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- honeycomb
- honeycomb structure
- raw material
- particles
- fired body
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Abstract
本发明提供蜂窝结构体的制造方法,该蜂窝结构体的机械强度优异。一种蜂窝结构体的制造方法,其是包含蜂窝烧制体的蜂窝结构体的制造方法,该蜂窝烧制体中,2个以上的贯通孔隔着隔壁在长度方向并列设置,其特征在于,其包括下述工序:原料混合工序,制作包含二氧化铈‑氧化锆复合氧化物颗粒、氧化铝颗粒、无机粘结剂和无机纤维的原料糊料;成型工序,通过将上述原料糊料成型而制作出2个以上的贯通孔隔着隔壁在长度方向并列设置的蜂窝成型体;干燥工序,将通过成型工序成型出的蜂窝成型体进行干燥;以及烧制工序,对通过干燥工序干燥后的蜂窝成型体进行烧制,由此制作出蜂窝烧制体;在原料混合工序中,将上述无机粘结剂与上述无机纤维进行预混合。
Description
技术领域
本发明涉及蜂窝结构体的制造方法。
背景技术
从汽车等内燃机中排出的尾气中包含一氧化碳(CO)、氮氧化物(NOx)、烃(HC)等有害气体和颗粒状物质(PM)。对这样的有害气体进行分解的尾气净化催化剂也被称为三元催化剂,通常为将包含具有催化活性的贵金属颗粒的浆料洗涂至由堇青石等构成的蜂窝状的整体式基材而设有催化剂层的催化剂。
另一方面,专利文献1中公开了一种蜂窝结构体的制造方法,该方法中,将包含二氧化铈-氧化锆复合氧化物颗粒(以下也称为CZ颗粒)、氧化铝颗粒、无机纤维和无机粘结剂的原料糊料进行挤出成型,将所得到的挤出成型体进行干燥、烧制,由此制造出蜂窝结构体。
现有技术文献
专利文献
专利文献1:国际公开第2018/012565号
发明内容
发明所要解决的课题
但是,专利文献1所记载的方法中具有蜂窝结构体的机械强度不充分的问题。
发明人针对上述问题进行了深入研究,结果发现,在将蜂窝结构体三点弯曲而使其破损的情况下,在断裂面中存在无机纤维被拔出而得到的痕迹,因此推测出,作为增强材料添加的无机纤维与其他材料的结合强度低为该机械强度不充分的原因。
本发明是为了解决上述课题而完成的发明,本发明的目的在于提供机械强度优异的蜂窝结构体的制造方法。
用于解决课题的手段
本发明的蜂窝结构体的制造方法是包含蜂窝烧制体的蜂窝结构体的制造方法,该蜂窝烧制体中,2个以上的贯通孔隔着隔壁在长度方向并列设置,该方法的特征在于,其包括下述工序:原料混合工序,在该工序中,制作包含二氧化铈-氧化锆复合氧化物颗粒、氧化铝颗粒、无机粘结剂和无机纤维的原料糊料;成型工序,在该工序中,通过将上述原料糊料成型而制作出2个以上的贯通孔隔着隔壁在长度方向并列设置的蜂窝成型体;干燥工序,在该工序中,将通过上述成型工序成型出的蜂窝成型体进行干燥;以及烧制工序,在该工序中,对通过上述干燥工序干燥后的蜂窝成型体进行烧制,由此制作出蜂窝烧制体,上述原料混合工序中,将上述无机粘结剂与上述无机纤维进行预混合。
在将无机粘结剂和无机纤维与其他材料一次性混合时,无机粘结剂优先附着在比表面积大的CZ颗粒、氧化铝颗粒的表面,在无机纤维的表面不容易附着无机粘结剂。因此认为,无机纤维与无机粘结剂的结合不充分,无机纤维的结合强度降低。
与之相对,在本发明的蜂窝结构体的制造方法中,在原料混合工序中,将无机粘结剂与无机纤维预混合。
据认为,通过将无机粘结剂与无机纤维预混合,能够增加存在于无机纤维的表面的无机粘结剂的量,能够增加无机纤维与其他材料的结合强度。
需要说明的是,无机纤维是指长径比为5以上的无机纤维。
本发明的蜂窝结构体的制造方法中,上述无机粘结剂优选为勃姆石。
勃姆石是以AlOOH的组成来表示的氧化铝一水合物,其在水等介质中良好地分散,因此本发明的蜂窝结构体的制造方法中,优选使用勃姆石作为无机粘结剂。
本发明的蜂窝结构体的制造方法中,上述无机纤维优选为氧化铝纤维。
无机纤维为氧化铝纤维时,蜂窝结构体的耐热性提高。
本发明的蜂窝结构体的制造方法中,在上述原料混合工序中,上述二氧化铈-氧化锆复合氧化物颗粒相对于上述氧化铝颗粒的重量比(二氧化铈-氧化锆复合氧化物颗粒/氧化铝颗粒)优选为1.0~3.0。
上述重量比(二氧化铈-氧化锆复合氧化物颗粒/氧化铝颗粒)为1.0~3.0时,二氧化铈-氧化锆复合氧化物颗粒的含量高,该二氧化铈-氧化锆复合氧化物颗粒可作为助催化剂使用,因此尾气的净化性能提高。
本发明的蜂窝结构体的制造方法中优选进一步包括在上述蜂窝烧制体中负载贵金属的负载工序。
通过在蜂窝烧制体中负载贵金属,能够用于尾气净化用途。
附图说明
图1是示意性示出通过本发明的蜂窝结构体的制造方法得到的蜂窝结构体的一例的立体图。
图2是实施例1的蜂窝结构体的破坏断面的SEM图像。
图3是比较例1的蜂窝结构体的破坏断面的SEM图像。
具体实施方式
[蜂窝结构体]
首先对通过本发明的蜂窝结构体的制造方法得到的蜂窝结构体进行说明。
图1是示意性示出通过本发明的蜂窝结构体的制造方法得到的蜂窝结构体的一例的立体图。
图1所示的蜂窝结构体10具备2个以上的贯通孔12隔着隔壁13在长度方向(图1中由双箭头L表示的方向)并列设置的单一的蜂窝烧制体11。蜂窝烧制体11包含CZ颗粒和氧化铝颗粒,具有挤出成型体的形状。
如图1所示,蜂窝结构体10由单一的蜂窝烧制体11构成的情况下,蜂窝结构体10也是蜂窝烧制体本身。
蜂窝结构体中,蜂窝烧制体由CZ颗粒、氧化铝颗粒、无机粘结剂和无机纤维构成。
如下文所述,蜂窝烧制体是通过将包含CZ颗粒、氧化铝颗粒、无机粘结剂和无机纤维的原料糊料挤出成型后进行烧制而制作出的。
本发明的蜂窝结构体是否具有CZ颗粒和氧化铝颗粒可以通过X射线衍射(XRD)来确认。
蜂窝结构体可以具备单一的蜂窝烧制体,也可以具备多个蜂窝烧制体,多个蜂窝烧制体可以通过粘接剂进行结合。
蜂窝结构体中,在蜂窝烧制体的外周面可以形成外周涂层。
蜂窝结构体中,上述蜂窝烧制体的气孔率优选为45~70体积%。
蜂窝烧制体的气孔率为45~70体积%时,能够兼顾高机械强度和尾气净化性能。
上述蜂窝烧制体的气孔率小于45体积%时,在隔壁中,能够有助于气体向内部的扩散的气孔的比例减少,尾气净化性能可能会降低。另一方面,上述蜂窝烧制体的气孔率大于70体积%时,由于气孔率过高,因而蜂窝结构体的机械特性劣化,蜂窝结构体在使用中容易发生裂纹或破坏等。
蜂窝烧制体的气孔率可以通过以下说明的重量法进行测定。
(1)将蜂窝烧制体切割成10孔道×10孔道×10mm的尺寸,作为测定试样。将该测定试样使用离子交换水和丙酮进行超声波清洗后,使用烘箱在100℃进行干燥。需要说明的是,10孔道×10孔道×10mm的测定试样是指按照下述方式切割而成的试样:以贯通孔纵向排列10个、横向排列10个的状态,包括最外侧的贯通孔和构成该贯通孔的隔壁,长度方向的长度为10mm。
(2)使用测定显微镜(尼康制Measuring Microscope MM-40倍率:100倍),对测定试样的截面形状的尺寸进行测定,根据几何学的计算求出体积(需要说明的是,在无法由几何学的计算求出体积的情况下,实测水饱和重量和水中重量来进行体积测定)。
(3)根据由计算求出的体积和由比重计测定得到的测定试样的真密度,计算出假定测定试样为完全的致密体的情况下的重量。需要说明的是,利用比重计进行的测定过程如(4)所示。
(4)将蜂窝烧制体粉碎,准备23.6cc的粉末。将所得到的粉末在200℃下干燥8小时。之后使用Micromeritics公司制造的Auto Pycnometer1320,依据JIS R 1620(1995)测定真密度。设排气时间为40分钟。
(5)采用电子天平(A&D制HR202i)对测定试样的实际重量进行测定。
(6)根据下式求出蜂窝烧制体的气孔率。
(蜂窝烧制体的气孔率)=100-(测定试样的实际的重量/假定测定试样为完全的致密体的情况下的重量)×100[%]
需要说明的是,即使在本发明的蜂窝结构体中直接负载贵金属的情况下,由贵金属负载所致的蜂窝烧制体的气孔率的变化也小到可以忽略不计。
构成蜂窝结构体的氧化铝颗粒优选为θ相的氧化铝颗粒。
氧化铝颗粒为θ相的氧化铝颗粒时,耐热性高,因而即使在负载贵金属并长时间使用后也能够发挥出高尾气净化性能。
无机粘结剂的含有比例优选为0.1~10重量%,无机纤维的含有比例优选为10~40重量%。
作为蜂窝结构体的形状,并不限于圆柱状,可以举出棱柱状、椭圆柱状、长圆柱状、带圆倒角的棱柱状(例如,带圆倒角的三棱柱状)等。
蜂窝结构体中,作为蜂窝烧制体的贯通孔的形状,并不限于四棱柱状,可以举出三棱柱状、六棱柱状等。
蜂窝结构体中,蜂窝烧制体的垂直于长度方向的截面的贯通孔的密度优选为31~155个/cm2。
蜂窝结构体中,蜂窝烧制体的隔壁的厚度优选为0.05~0.50mm、更优选为0.10~0.30mm。
蜂窝结构体中,在蜂窝烧制体的外周面形成有外周涂层的情况下,外周涂层的厚度优选为0.1~2.0mm。
蜂窝结构体可以具备单一的蜂窝烧制体,也可以具备多个蜂窝烧制体,多个蜂窝烧制体可以利用粘接剂结合。
蜂窝结构体中,优选在上述蜂窝烧制体中负载有贵金属。
上述蜂窝结构体中,在上述蜂窝烧制体中负载有起到作为催化剂的功能的贵金属时,也可以作为尾气净化用的蜂窝催化剂使用。
作为贵金属,例如可以举出铂、钯、铑等。
蜂窝结构体中,贵金属的负载量优选为0.1~15g/L、更优选为0.5~10g/L。
本说明书中,贵金属的负载量是指蜂窝结构体的单位表观体积的贵金属的重量。需要说明的是,蜂窝结构体的表观体积是包含空隙体积在内的体积,其包含外周涂层和/或粘接层的体积。
[蜂窝结构体的制造方法]
接着对本发明的蜂窝结构体的制造方法进行说明。
本发明的蜂窝结构体的制造方法是包含蜂窝烧制体的蜂窝结构体的制造方法,该蜂窝烧制体中,2个以上的贯通孔隔着隔壁在长度方向并列设置,其特征在于,该制造方法包括下述工序:原料混合工序,在该工序中,制作包含二氧化铈-氧化锆复合氧化物颗粒、氧化铝颗粒、无机粘结剂和无机纤维的原料糊料;成型工序,在该工序中,通过将上述原料糊料成型而制作出2个以上的贯通孔隔着隔壁在长度方向并列设置的蜂窝成型体;干燥工序,在该工序中,将通过上述成型工序成型出的蜂窝成型体进行干燥;以及烧制工序,在该工序中,对通过上述干燥工序干燥后的蜂窝成型体进行烧制,由此制作出蜂窝烧制体,上述原料混合工序中,将上述无机粘结剂与上述无机纤维进行预混合。
(原料混合工序)
在原料混合工序中,制作包含CZ颗粒、氧化铝颗粒、无机粘结剂和无机纤维的原料糊料,此时,将无机粘结剂与无机纤维预混合。
作为构成无机纤维的材料没有特别限定,例如可以举出氧化铝、二氧化硅、碳化硅、氧化硅-氧化铝、玻璃、钛酸钾、硼酸铝等,也可以将两种以上合用。这些之中,优选氧化铝。
无机粘结剂没有特别限定,可以举出氧化铝溶胶、硅溶胶、二氧化钛溶胶、水玻璃、海泡石、凹凸棒石、勃姆石等中包含的固体成分,这些无机粘结剂也可以将两种以上合用。它们之中,优选勃姆石。
勃姆石是以AlOOH的组成来表示的氧化铝一水合物,其在水等介质中良好地分散,因此本发明的蜂窝结构体的制造方法中,优选使用勃姆石作为粘结剂。
无机粘结剂与无机纤维的预混合可以使用混合器、超微磨碎机等,也可以使用捏合机等。另外,可以根据需要添加分散介质。作为分散介质没有特别限定,可以举出水、苯等有机溶剂、甲醇等醇等,也可以将两种以上合用。
此外还可以添加表面活性剂等助剂。
将无机粘结剂与无机纤维预混合后,进一步混合CZ颗粒和氧化铝颗粒,得到原料糊料。
作为氧化铝颗粒,优选使用其平均粒径为1~30μm的颗粒。
另外,作为CZ颗粒,优选使用其平均粒径为1~10μm的颗粒。
此外,所使用的氧化铝颗粒的平均粒径优选大于CZ颗粒的平均粒径。
需要说明的是,CZ颗粒和氧化铝颗粒的平均粒径可以通过激光衍射式粒度分布测定装置(MALVERN公司制造MASTERSIZER2000)来求出。
制备上述原料糊料时所使用的上述二氧化铈-氧化锆复合氧化物颗粒相对于上述氧化铝颗粒的重量比(二氧化铈-氧化锆复合氧化物颗粒/氧化铝颗粒)优选为1.0~3.0。
上述重量比(二氧化铈-氧化锆复合氧化物颗粒/氧化铝颗粒)为1.0~3.0时,二氧化铈-氧化锆复合氧化物颗粒的含量高,该二氧化铈-氧化锆复合氧化物颗粒可作为助催化剂使用,因此尾气的净化性能提高。
作为制备原料糊料时所使用的氧化铝颗粒,优选θ相的氧化铝颗粒。
作为制备原料糊料时所使用的其他原料,可以举出有机粘结剂、造孔剂、成型助剂、分散介质等。
作为有机粘结剂没有特别限定,可以举出甲基纤维素、羧甲基纤维素、羟基乙基纤维素、聚乙二醇、酚树脂、环氧树脂等,也可以将两种以上合用。
作为分散介质没有特别限定,可以举出水、苯等有机溶剂、甲醇等醇等,也可以将两种以上合用。
作为上述造孔剂,例如可以举出丙烯酸类树脂、淀粉、碳等。
造孔剂的平均粒径没有特别限定,优选为10~60μm。
造孔剂的平均粒径与氧化铝颗粒和CZ颗粒的平均粒径同样地可以使用激光衍射式粒度分布测定装置(MALVERN公司制造MASTERSIZER2000)进行测定。
作为成型助剂没有特别限定,可以举出乙二醇、糊精、脂肪酸、脂肪酸皂、多元醇等,也可以将两种以上合用。
在使用CZ颗粒、氧化铝颗粒、无机纤维和无机粘结剂作为上述的原料时,关于它们的混合比例,相对于原料中的烧制工序后残留的总固体成分,优选CZ颗粒为40~60重量%、氧化铝颗粒为15~35重量%、无机纤维为10~40重量%、无机粘结剂为0.1~10重量%。
造孔剂的干燥体积在上述原料糊料的干燥体积中所占的比例优选为45~70体积%。
另外,制备原料糊料时所使用的CZ颗粒相对于氧化铝颗粒的重量比(CZ颗粒/氧化铝颗粒)优选为1.0~3.0。
重量比(CZ颗粒/氧化铝颗粒)为1.0~3.0时,CZ颗粒的含量高,由于该CZ颗粒可作为助催化剂使用,因此能够增强所负载的催化剂的催化作用,能够进一步提高作为蜂窝催化剂的性能。
在制备原料糊料时,优选进行混合混炼,可以使用混合器、超微磨碎机等进行混合,可以使用捏合机等进行混炼。
(成型工序)
在成型工序中,通过对由原料混合工序得到的原料糊料进行成型而制作出2个以上的贯通孔隔着隔壁在长度方向并列设置的蜂窝成型体。
原料糊料可通过例如挤出成型等方法进行成型。
具体地说,使该原料糊料通过规定形状的模具,由此形成具有规定形状的贯通孔的蜂窝成型体的连续体,通过将其切割成规定的长度而制成蜂窝成型体。
(干燥工序)
在本发明的蜂窝结构体的制造方法中,将通过上述成型工序而成型得到的成型体进行干燥。
此时,优选使用微波干燥机、热风干燥机、高频干燥机、减压干燥机、真空干燥机、冷冻干燥机等干燥机,对蜂窝成型体进行干燥,制作出蜂窝干燥体。
本说明书中,也将进行烧制工序之前的蜂窝成型体和蜂窝干燥体统称为蜂窝成型体。
(烧制工序)
在烧制工序中,对通过干燥工序干燥后的成型体进行烧制,由此制作出蜂窝烧制体。需要说明的是,由于该工序进行蜂窝成型体的脱脂和烧制,因此也可以将其称为“脱脂·烧制工序”,但方便起见将其称为“烧制工序”。
烧制工序的温度优选为800~1300℃、更优选为900~1200℃。另外,烧制工序的时间优选为1~24小时、更优选为3~18小时。烧制工序的气氛没有特别限定,优选氧浓度为1~20%。
通过以上的工序可以制造出本发明的蜂窝结构体。
(其他工序)
本发明的蜂窝结构体的制造方法可以根据需要进一步包括在上述蜂窝烧制体中负载贵金属的负载工序。
作为在蜂窝烧制体中负载贵金属的方法,例如可以举出将蜂窝烧制体或蜂窝结构体浸渍在包含贵金属颗粒或络合物的溶液中,之后将其拉起并进行加热的方法等。
在蜂窝结构体具备外周涂层的情况下,可以在形成外周涂层之前的蜂窝烧制体中负载贵金属,也可以在形成了外周涂层之后的蜂窝烧制体或蜂窝结构体中负载贵金属。
本发明的蜂窝结构体的制造方法中,由上述负载工序负载的贵金属的负载量优选为0.1~15g/L、更优选为0.5~10g/L。
本发明的蜂窝结构体的制造方法中,在蜂窝烧制体的外周面形成外周涂层的情况下,外周涂层可以通过在蜂窝烧制体的除两端面以外的外周面涂布外周涂层用糊料,之后进行干燥固化来形成。作为外周涂层用糊料,可以举出与原料糊料相同组成的糊料。
(实施例)
以下示出进一步具体公开本发明的实施例。需要说明的是,本发明并不仅限于以下的实施例。
[评价用样品的制作]
(实施例1)
首先,将氧化铝纤维(平均纤维径:3μm、平均纤维长:60μm)10.6重量%、作为无机粘结剂的勃姆石2.8重量%和离子交换水10.0重量%预混合10分钟。
接着,添加CZ颗粒(平均粒径:2μm)16.9重量%、γ氧化铝颗粒(平均粒径:2μm)8.5重量%、作为有机粘结剂的甲基纤维素3.9重量%、作为造孔剂的丙烯酸类树脂(平均粒径:32μm)28.1重量%、作为成型助剂的表面活性剂聚氧乙烯油基醚2.9重量%和离子交换水16.2重量%,进一步进行混合混炼,制备原料糊料。
需要说明的是,γ氧化铝颗粒、CZ颗粒和造孔剂的平均粒径使用激光衍射式粒度分布测定装置(MALVERN公司制造MASTERSIZER2000)进行测定。
使用挤出成型机,对原料糊料进行挤出成型,制作圆柱状的蜂窝成型体。之后,在使用减压微波干燥机将蜂窝成型体以输出功率1.74kW、减压6.7kPa的条件干燥12分钟后,在1100℃进行10小时的脱脂·烧制,由此制作出蜂窝烧制体。蜂窝烧制体是直径为103mm、长度为80mm的圆柱状,贯通孔的密度为77.5个/cm2(500cpsi)、隔壁的厚度为0.127mm(5mil)。
(比较例1)
除了将制备原料糊料的原料全部一次性混合以外,利用与实施例1相同的过程制造比较例1的蜂窝结构体。
[3点弯曲强度的测定和破坏断面的观察]
首先,作为3点弯曲强度测定用样品,将以与实施例1和比较例1相同的配比进行混合、混炼得到的原料糊料成型为长方体,在相同条件下进行脱脂、烧制后加工成6mm×6mm×40mm而得到部件,准备10件这样的部件,作为3点弯曲强度测定用样品(以下称为样品)。相对于样品的主面(样品的外周面中的较宽的一面)在垂直方向施加负荷,对破坏负荷(样品被破坏的负荷)进行测定。对于10件3点弯曲强度测定用样品进行破坏负荷的测定,将其平均值作为弯曲强度。3点弯曲强度试验参考JIS R1601,使用INSTRON5582,以跨矩30mm、速度1mm/min进行测定。3点弯曲强度在实施例1中为6.9MPa、在比较例1中为5.2MPa。
此外通过SEM对由于破坏而露出的样品的表面(破坏断面)进行观察。将结果示于图2和图3中。图2是实施例1的蜂窝结构体的破坏断面的SEM图像,图3是比较例1的蜂窝结构体的破坏断面的SEM图像。
由图2和图3的结果确认到,实施例1的样品中,破坏断面中氧化铝纤维未从基材中拔出,而比较例1的样品中,破坏断面中氧化铝纤维呈拔出的状态。因此可知,利用本发明的蜂窝结构体的制造方法得到的蜂窝结构体中,氧化铝纤维与其他材料的接合性良好,显示出优异的机械强度。
符号的说明
10 蜂窝结构体
11 蜂窝烧制体
12 贯通孔
13 隔壁
Claims (5)
1.一种蜂窝结构体的制造方法,其是包含蜂窝烧制体的蜂窝结构体的制造方法,该蜂窝烧制体中,2个以上的贯通孔隔着隔壁在长度方向并列设置,其特征在于,
该制造方法包括下述工序:
原料混合工序,在该工序中,制作包含二氧化铈-氧化锆复合氧化物颗粒、氧化铝颗粒、无机粘结剂和无机纤维的原料糊料;
成型工序,在该工序中,通过将所述原料糊料成型而制作出蜂窝成型体,该蜂窝成型体中,2个以上的贯通孔隔着隔壁在长度方向并列设置;
干燥工序,在该工序中,将通过所述成型工序成型出的蜂窝成型体进行干燥;以及
烧制工序,在该工序中,对通过所述干燥工序干燥后的蜂窝成型体进行烧制,由此制作出蜂窝烧制体,
所述原料混合工序中,将所述无机粘结剂与所述无机纤维进行预混合。
2.如权利要求1所述的蜂窝结构体的制造方法,其中,所述无机粘结剂为勃姆石。
3.如权利要求1或2所述的蜂窝结构体的制造方法,其中,所述无机纤维为氧化铝纤维。
4.如权利要求1~3中任一项所述的蜂窝结构体的制造方法,其中,所述原料混合工序中,所述二氧化铈-氧化锆复合氧化物颗粒相对于所述氧化铝颗粒的重量比、即二氧化铈-氧化锆复合氧化物颗粒/氧化铝颗粒为1.0~3.0。
5.如权利要求1~4中任一项所述的蜂窝结构体的制造方法,其中,该制造方法进一步包括在所述蜂窝烧制体中负载贵金属的负载工序。
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