CN1167509C - 陶瓷蜂窝状催化剂载体及其制备方法 - Google Patents
陶瓷蜂窝状催化剂载体及其制备方法 Download PDFInfo
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Abstract
一种陶瓷蜂窝状催化剂载体，其特征在于：所述催化剂载体具有20%或更低的孔隙率、隔墙平均表面糙度Ra具有0.5μm或更大的较大值；一种制备陶瓷蜂窝状催化剂载体的方法，所述方法包括通过将陶瓷材料成形并随后干燥而提供干燥的陶瓷蜂窝，将所述干燥的陶瓷蜂窝暴露于其中含有磨料粒的气流中，从而使其隔墙表面粗糙化，随后将所述干燥的陶瓷蜂窝烧结，或者所述方法包括通过将陶瓷材料成形并随后进行干燥和烧结而提供已烧结的陶瓷蜂窝，随后将所得的已烧结的陶瓷蜂窝暴露于其中含有磨料粒的气流或水流中，从而使已烧结的陶瓷蜂窝的隔墙表面粗糙化。
Description
技术领域
本发明涉及用于净化汽车等排出的废气的陶瓷蜂窝状催化剂载体及其制备方法。
技术背景
陶瓷蜂窝状催化剂载体用于固定净化汽车等排出的废气的催化剂。通常，陶瓷蜂窝状催化剂载体具有大量的各具有许多细孔的隔墙，在这些隔墙上涂布了具有高比表面积的γ-氧化铝及催化剂，由此用于汽车等中。鉴于近期加强废气管理，这就要求将陶瓷蜂窝状催化剂载体的隔墙厚度制备得薄一些以提高催化剂性能和发动机性能。
然而，如果将所述陶瓷蜂窝状催化剂载体的隔墙制成薄得如上所述，则降低了所述陶瓷蜂窝状催化剂载体的机械强度。为了消除这样的问题，例如在日本专利公开公布号10-174885(JP-A-10-174885)中公开了一项技术，该技术通过控制原材料滑石的尺寸和CaO的量获得了具有高强度和孔隙率为18％或更低的紧密堇青石。然而，如果降低了孔隙率，虽然可以提高强度，但这将出现新的问题，如劣化了具有高比表面积的γ-氧化铝及催化剂的可涂布性。
发明公开
本发明一个目的是消除上述缺点并提供即使隔墙很薄，仍具有作为催化剂载体的足够强度和优异的催化剂可涂布性的陶瓷蜂窝状载体及其制备方法。
本发明的陶瓷蜂窝状催化剂载体的特征在于孔隙率为20％或更低、载体隔墙的平均表面糙度Ra为0.5μm或更高。
并且，本发明第一方面涉及一种制备方法，一种制备上述陶瓷蜂窝状催化剂载体的方法，所述方法包含以下步骤：将陶瓷原材料成形以得到陶瓷蜂窝状坯体；干燥所述陶瓷蜂窝状坯体以得到陶瓷蜂窝状干缩坯体；通过将所述陶瓷蜂窝状干缩坯体暴露在含有抛光粉末的气流中，使其隔离墙粗糙化；以及在表面处理后烧结所述陶瓷蜂窝状干缩坯体。
此外，本发明第二方面涉及一种制备方法，一种制备上述陶瓷蜂窝状催化剂载体的方法，所述方法包含以下步骤：将陶瓷原材料成形以获得陶瓷蜂窝状坯体；干燥并烧结所述陶瓷蜂窝状坯体以得到陶瓷蜂窝状烧结体；通过将所述陶瓷蜂窝状烧结体暴露在含有抛光粉末的气流或水流中，使其隔墙粗糙化。
在本发明中，通过在成形和干燥陶瓷原料之后或进一步在烧结成形的坯体之后对隔墙的表面进行表面处理，优选用抛光粉末(如氧化铝和金刚石)的方式进行处理可得到具有孔隙率为20％或更低和载体隔墙经过粗糙化后具有平均表面糙度(Ra)为0.5μm或更高的陶瓷蜂窝状催化剂载体。如此，发现可获得具有高强度和优异的γ-氧化铝或催化剂可涂布性的陶瓷蜂窝状催化剂载体。
在本发明中，规定平均表面糙度为0.5μm或更高的原因是如果小于0.5μm，则γ-氧化铝和催化剂无法充分涂布在其上面。此外，规定孔隙率为20％或更低的原因是如果大于20％，则不能获得足够的强度。此外，上述表面处理可通过用泵的方式循环其中分散有抛光粉末(如氧化铝和金钢石)的液体来实施，或通过将陶瓷蜂窝暴露在其中包含有抛光粉末的空气流中一段规定的时间来实施。而且，作为所述陶瓷蜂窝状催化剂载体的原材料除了堇青石外，通常还采用普通陶瓷如局部稳定的氧化锆、四氮化三硅、氧化铝、碳化硅和磷酸锆。
附图的简要描述
图1是解释本发明第一方面的制备陶瓷蜂窝状催化剂载体的方法的流程图；
图2是解释本发明第二方面的制备陶瓷蜂窝状催化剂载体的方法的流程图。
实施本发明的最佳方式
图1是解释本发明第一方面的制备陶瓷蜂窝状催化剂载体的方法的流程图。下文将参考图1进行说明。首先，将陶瓷原材料成形以得到陶瓷蜂窝状坯体，干燥所述陶瓷蜂窝状坯体以得到陶瓷蜂窝状干缩坯体，然后，对所述陶瓷蜂窝状干缩坯体进行表面处理。根据本发明第二方面的制备方法的表面处理通过将所述陶瓷蜂窝状干缩坯体暴露在其中含有如氧化铝、金刚石等抛光粉末的气流中一段规定的时间实施，然后，将所述经过表面处理的陶瓷蜂窝状干缩坯体烧结。如此，可以获得本发明的具有孔隙率为20％或更低和载体隔墙的平均表面糙度(Ra)为0.5μm或更高的陶瓷蜂窝状催化剂载体。
图2是解释本发明第二方面的制备陶瓷蜂窝状催化剂载体的方法的流程图。下文将参考图2进行说明。首先，将陶瓷原材料成形以获得陶瓷蜂窝状坯体，干燥并烧结所述陶瓷蜂窝状坯体以得到陶瓷蜂窝状烧结体。然后，对所述陶瓷蜂窝状烧结体进行表面处理。根据本发明第一方面的制备方法的表面处理通过用泵的方式循环其中分散有抛光粉末(如氧化铝和金钢石)的液体实施，或通过将陶瓷蜂窝暴露在其中包含有抛光粉末的空气流的气氛中一段规定的时间实施。如此，可获得本发明的具有孔隙率为20％或更低和载体隔墙的平均表面糙度(Ra)为0.5μm或更高的陶瓷蜂窝状催化剂载体。
应注意的是，使用众所周知的制备孔隙率为20％或更低的载体的方法。如可以使用日本专利公开公布号10-174885(JP-A-10-174885)中所公开的方法，该方法规定了原材料滑石的尺寸和CaO的量。此外，在如此获得的本发明的陶瓷蜂窝状催化剂载体中，优选隔墙的厚度为60μm或更薄和蜂窝状坯体的开孔率(opening rate)为88％或更高。而且，优选陶瓷蜂窝状催化剂载体具有500kPa或更高的ISO强度。此外，如果隔墙表面的平均表面糙度为1.0μm或更高，则还可获得优异的可涂布性。因此，这也是一个优选的实施方案。
下文将对实际的实验进行说明。
根据下面的方法，通过制备蜂窝状载体并对所述蜂窝状载体进行表面处理得到陶瓷蜂窝状催化剂载体。随后，测量如此获得的陶瓷蜂窝状催化剂载体的孔隙率、弯曲强度、静压破裂强度、表面糙度和涂布量。本发明实施例和不在本发明范围内的对比实施例的结果显示在下表1中。
蜂窝状载体的制备
将原材料如滑石、氧化铝、高岭土混合以获得含有堇青石组分的混合物。然后，往所述混合物中加入适量用作微孔控制剂的粉碎的堇青石、水溶性纤维衍生物、表面活性剂和水以获得一批料。然后，根据已知的制备方法，对该批料进行捏和(kneeding)、炼泥(pugging)、挤压成形、干燥和烧结以获得含有堇青石组分的陶瓷蜂窝状催化剂载体，其隔墙厚度如表1所示。
蜂窝状载体的表面处理
在一个可打开和关闭的管中安装一个耐水风扇，以下述方式将所述陶瓷蜂窝状烧结体置于管中：使由隔墙确定的贯穿孔按风扇的水流方向排列。然后，通过风扇使水流通过所述陶瓷蜂窝状烧结体。在这种情况下，金刚石抛光粉末分散于风扇和所述陶瓷蜂窝状烧结体之间，从而蚀刻所述陶瓷蜂窝状烧结体的隔墙表面。在蚀刻加工之后，将所述陶瓷蜂窝状烧结体充分清洗和干燥以获得陶瓷蜂窝状催化剂载体。收集所述金刚石抛光粉末以循环使用。
孔隙率
根据汞注射方法测量如此获得的陶瓷蜂窝状催化剂载体的总微孔量以计算孔隙率。堇青石的真密度假定为2.52g/cm3。通过微晶学的AutoPore9405进行所述测量。
弯曲强度
根据上述蜂窝状载体同样的制备方法获得具有宽度为30mm、厚度为7mm和长度为150mm的堇青石平板。在这种情况下，在烧结和机械加工后，对所述平板进行表面处理。在完成所有加工后，根据JIS R1601测量五个样品的四点弯曲强度。
静压破裂强度
将如此获得的蜂窝状催化剂载体***到一个可弯曲的管中，对其施加水压静压。然后测量发生局部断裂的压力(kPa)。各种样品的数量分别为十个。
表面糙度
用Taylor-Hobson Company制造的FTS-S4C测量如此获得的陶瓷蜂窝状催化剂载体隔墙的平均表面糙度(Ra)。计算方法参考JISB0601，使用2μm的圆锥形金刚石做成尖端测试部分。
涂布量
表明如此获得的陶瓷蜂窝状催化剂载体的可涂布性的涂布量(g/每立方厘米陶瓷蜂窝状催化剂载体)如下进行测量：从陶瓷蜂窝状催化剂载体中切下尺寸为100mm×100mm×100mm的样品。同时按60∶40的比例混合5％的氧化铝-硝酸盐溶胶和γ-氧化铝制备氧化铝泥浆。然后，将所述样品浸入所述氧化铝泥浆中一段预定的时间。之后，将涂有所述氧化铝泥浆的样品干燥并在600℃下老化一小时。根据在涂布氧化铝泥浆的前后重量的增加计算表明可涂布性的涂布量(g/每平方厘米陶瓷蜂窝状催化剂载体)。
表1
| 本发明实施例 | 对比实施例 | |||||
| 1 | 2 | 3 | 4 | 1 | 2 | |
| 表面处理 | 有 | 有 | 有 | 有 | 无 | 无 |
| 载体隔墙厚度(μm) | 50 | 60 | 50 | 50 | 50 | 50 |
| 载体孔隙率(％) | 18 | 18 | 18 | 20 | 32 | 20 |
| 表面糙度(μm) | 2.0 | 1.5 | 0.5 | 0.7 | 1.9 | 0.3 |
| 弯曲强度(MPa) | 42 | 42 | 43 | 38 | 21 | 40 |
| 静压破裂强度(kPa) | 1370 | 1450 | 1380 | 1180 | 590 | 1200 |
| 涂布量(g/每平方厘米蜂窝状催化剂载体) | 0.20 | 0.17 | 0.10 | 0.13 | 0.25 | 0.05 |
从表1显示的结果可有如下理解：首先，在本发明的实施例1中，当实施了表面处理和表面糙度为2.0μm时，可以获得高涂布量和低孔隙率，因此可获得高的强度。当降低表面糙度，涂布量以如下方式降低：当表面糙度为0.5μm时，涂布量为0.1g/每立方厘米蜂窝状催化剂载体(本发明的实施例3)。如对比实施例2显示，当涂布量减少到0.05g/每立方厘米蜂窝状催化剂载体的水平时，必须一次又一次地重复涂布过程才能获得产品必须的足够涂布量，因此这是不优选的。由本发明的实施例2和实施例4可看出，减少隔墙厚度和提高孔隙率导致了强度的降低。当孔隙率如对比实施例1中显示非常高时，表面糙度提高并同时涂布量也变得很高。然而，静压破裂强度很低。
从上述的结果中发现从本发明的实施例1-4中可获得足够的弯曲强度、足够的静压破裂强度和足够的涂布量，其中载体的孔隙率为20％或更低、表面糙度为0.5μm或更高，而在对比实施例1或2中强度或涂布量是不足够的，其中孔隙率或表面糙度二者中任一个的条件是不能令人满意的。
在本发明的实施例1-4中，对所述陶瓷蜂窝状烧结体进行表面处理以获得陶瓷蜂窝状催化剂载体，但以对陶瓷蜂窝状的干燥坯体进行表面处理的方式可获得同样结果的陶瓷蜂窝状催化剂载体。
工业适用性
从上述说明可清楚地理解到，本发明的具有孔隙率为20％或更低、载体的隔墙经过粗糙化后具有平均表面糙度(Ra)为0.5μm或更高的陶瓷蜂窝状催化剂载体可通过对所示隔墙表面进行表面处理而获得，优选采用抛光粉末(如氧化铝和金刚石)在成型和干燥陶瓷原材料或进一步在烧结成型的坯体之后进行表面处理。因此，可以制得具有高强度和优异γ-氧化铝或催化剂可涂布性的陶瓷蜂窝状催化剂载体。
Claims (5)
1、一种陶瓷蜂窝状催化剂载体，其特征在于：所述催化剂载体的孔隙率为20％或更低、载体的隔墙的平均表面糙度(Ra)为0.5μm或更高，而所述的隔墙厚度为60μm或更薄。
2、权利要求1的陶瓷蜂窝状催化剂载体，其中所述载体包括堇青石组合物作为主要成分。
3、权利要求1的陶瓷蜂窝状催化剂载体，其中所述载体的隔墙的平均表面糙度(Ra)为1.0μm或更高。
4、一种制备权利要求1所阐述的陶瓷蜂窝状催化剂载体的方法，所述方法包含如下步骤：将陶瓷原材料成形以获得陶瓷蜂窝状坯体；干燥所述陶瓷蜂窝状坯体以获得陶瓷蜂窝状干缩坯体；通过将所述陶瓷蜂窝状干缩坯体暴露在含有抛光粉末的气流中，使其隔墙的表面粗糙化；以及在表面处理后烧结所述陶瓷蜂窝状干缩坯体。
5、一种制备权利要求1所阐述的陶瓷蜂窝状催化剂载体的方法，所述方法包含如下步骤：将陶瓷原材料成形以获得陶瓷蜂窝状坯体；干燥并烧结所述陶瓷蜂窝状坯体以获得陶瓷蜂窝状烧结体；通过将所述陶瓷蜂窝状干缩坯体暴露在含有抛光粉末气流或水流中，使其隔墙的表面粗糙化。
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| JP2004000901A (ja) * | 2002-03-29 | 2004-01-08 | Ngk Insulators Ltd | 多孔質ハニカム構造体 |
| JP2005254751A (ja) * | 2004-03-15 | 2005-09-22 | Ngk Insulators Ltd | セラミックスハニカム構造体の製造方法 |
| CN101395099A (zh) * | 2006-03-07 | 2009-03-25 | 日本碍子株式会社 | 陶瓷结构体及其制造方法 |
| RU2009132612A (ru) * | 2007-01-31 | 2011-03-10 | Басф Каталистс Ллк (Us) | Газовые катализаторы, включающие пористую сотовидную стенку |
| US20100237524A1 (en) * | 2007-04-25 | 2010-09-23 | Vicki Chen | Method of manufacturing ceramic capable of adsorbing fragrance and releasing fragrant aroma |
| KR101117468B1 (ko) * | 2008-05-20 | 2012-03-07 | 이비덴 가부시키가이샤 | 허니컴 구조체 |
| JP5916310B2 (ja) | 2011-07-26 | 2016-05-11 | 日本碍子株式会社 | ハニカム触媒担体 |
| US8865054B1 (en) * | 2013-03-15 | 2014-10-21 | Ibiden Co., Ltd. | Method for manufacturing aluminum-titanate-based ceramic honeycomb structure |
| US8974722B1 (en) * | 2013-03-15 | 2015-03-10 | Ibiden Co., Ltd. | Method for manufacturing aluminum-titanate-based ceramic honeycomb structure |
| CN103387377A (zh) * | 2013-07-17 | 2013-11-13 | 彭红 | 一种基于超大型蜂窝陶瓷载体拼接用的拼接泥 |
| JP6749853B2 (ja) * | 2017-01-31 | 2020-09-02 | 日本碍子株式会社 | ハニカム構造体の製造方法及びハニカム構造体 |
| CN111068704A (zh) * | 2018-10-19 | 2020-04-28 | 南京沿江资源生态科学研究院有限公司 | 一种用于热分解有机物的催化剂及其制备方法 |
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| WO2001060514A1 (fr) | 2001-08-23 |
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