CN110304937A - 一种蜂窝陶瓷过滤器载体及其制备方法 - Google Patents

一种蜂窝陶瓷过滤器载体及其制备方法 Download PDF

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CN110304937A
CN110304937A CN201910701890.1A CN201910701890A CN110304937A CN 110304937 A CN110304937 A CN 110304937A CN 201910701890 A CN201910701890 A CN 201910701890A CN 110304937 A CN110304937 A CN 110304937A
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silicon carbide
honeycomb filter
ceramic honeycomb
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李军虎
张金龙
田建刚
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Jincheng Fuji New Material Co Ltd
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Abstract

一种蜂窝陶瓷过滤器载体及其制备方法，本发明涉及蜂窝陶瓷技术领域；它由前驱体粉末和助剂组成，其中前驱体粉末与助剂的重量配比为85～90:10～15；其中，所述的前驱体粉末由如下重量份成分组成：碳化硅粗粉A40～70份、碳化硅微粉B 15～30份、高岭土3～5份、活性ɑ‑氧化铝微粉3～10份、硅微粉1～5份、石墨1～3份、造孔剂5～15份；所述的助剂由如下重量份成分组成：羟丙基甲基纤维素2～8份、硬脂酸盐1～4份、甘油2～6份、纳米铝溶胶液体5～15份、纯水25～30份。利用莫来石优越的热稳定性和碳化硅的导热性，可满足汽车尾气碳烟颗粒过滤使用。

Description

一种蜂窝陶瓷过滤器载体及其制备方法
技术领域
本发明涉及蜂窝陶瓷技术领域，具体涉及一种蜂窝陶瓷过滤器载体及其制备方法。
背景技术
目前，我国大气污染非常严重，汽车尾气排放污染占到了大气污染的70％以上。目前，国内已强制执行国Ⅴ标准，部分地区已执行国Ⅵ标准。因此要求汽车发动机厂家在尾气排放前对尾气进行催化处理。
蜂窝陶瓷是一种多孔性的功能材料，蜂窝陶瓷具有高的比表面积和良好的物理化学稳定性，另外还具有低密度、高渗透率、良好的能量吸收性能以及耐高温、耐腐蚀、化学稳定性和尺寸稳定性高、易于再生等诸多特点。
制备蜂窝陶瓷载体的材质除目前应用较为广泛的堇青石外，还有钛酸铝、碳化硅、莫来石等，其中碳化硅材料虽然其热膨胀系数相对偏高，但在一定程度上可以满足性能的要求，同时还具有强度高、耐高温、耐腐蚀、耐磨损、高比表面积、高比强等一系列优点。
现有技术采用重结晶碳化硅制备碳化硅质蜂窝陶瓷壁流式微粒过滤器(DPF)，但重结晶碳化硅制备需要采用真空气氛炉2450℃高温烧结，原材料需要高纯碳化硅原料，大大增加了碳化硅蜂窝陶瓷的售价。因此性价比更高的产品出现是本行业的一个重要技术难题。
发明内容
本发明的目的在于针对现有技术的缺陷和不足，提供一种结构简单，设计合理、使用方便的蜂窝陶瓷过滤器载体及其制备方法，利用莫来石优越的热稳定性和碳化硅的导热性，可满足汽车尾气碳烟颗粒过滤使用。
为实现上述目的，本发明所述的蜂窝陶瓷过滤器载体，它由前驱体粉末和助剂组成，其中前驱体粉末与助剂的重量配比为85～90:10～15；其中，所述的前驱体粉末由如下重量份成分组成：碳化硅粗粉A 40～70份、碳化硅微粉B 15～30份、高岭土3～5份、活性ɑ-氧化铝微粉3～10份、硅微粉1～5份、石墨1～3份、造孔剂5～15份；所述的助剂由如下重量份成分组成：羟丙基甲基纤维素2～8份、硬脂酸盐1～4份、甘油2～6份、纳米铝溶胶液体5～15份、纯水25～30份。
进一步地，所述的碳化硅粗粉A为SIC≥98.5，粒径D50＝30～50μm，FeO含量≤0.1％。
进一步地，所述的碳化硅微粉B为SIC≥98.5,粒径D50＝10～14μm，FeO含量≤0.1％。
进一步地，所述的活性ɑ-氧化铝微粉的粒径D50＝1～2μm，Na2O含量≤0.1％。
进一步地，所述的高岭土的粒径D50＝1～4μm。
进一步地，所述的硅微粉的粒径D50＝1～3μm，SiO2≥99％。
进一步地，所述的石墨的粒径D50＝1～5μm。
进一步地，所述的造孔剂为有机丙烯酸小球、淀粉、活性炭中的一种,粒径D50＝30～80μm。
进一步地，所述的羟丙基甲基纤维素为6000mpa.s。
本发明中所述的蜂窝陶瓷过滤器载体的制备方法，其操作步骤如下：
1、将碳化硅粗粉A、碳化硅微粉B、高岭土、活性ɑ-氧化铝微粉、硅微粉、石墨、造孔剂分别进行过筛处理，随后添加羟丙基甲基纤维素和硬脂酸盐，高速混合搅拌，得混合物；
2、向上述混合物中继续添加甘油、纳米铝溶胶液体和纯水，然后进行捏合、练泥、陈腐，最后挤出成型，形成毛坯；
3、将上述毛坯进行微波干燥、切割、烧成，烧成温度为1500-1600℃，再进行保温，保温过程中，对每个测温点进行实时测温，单独调整，保证炉内不同位置温度控制在0～5℃以内，保温时间为4-10小时，还原气氛，即制得蜂窝陶瓷载体；
4、将上述蜂窝陶瓷载体进行双面交叉堵孔、使同一孔道的孔一面开口一面封闭，再将多个蜂窝陶瓷载体进行拼接，构成一个新的载体，用外圆磨机加工成圆形载体，在圆形载体表面进行植皮，植皮后进行二次烧结，烧成温度1200-1300℃。
进一步地，所述的步骤4中拼接所采用的拼接料和植皮所采用的植皮料一致，均由如下质量百分比成分组成：碳化硅80-90％、纤维棉5-10％％、氧化铝10％、羟丙基甲基纤维素2％。
采用上述结构后，本发明有益效果为：
1、本发明通过对机动车尾气排放特点的研究，及市场上所售DPF载体性能测试，目前市场上所售DPF载体基本为重结晶碳化硅及堇青石质，使用温度分别为1600℃、1300℃；本发明为开发出一种介于两者之间使用温度的一种新型材料载体，材质为碳化硅复合莫来石质，利用莫来石优越的热稳定性和碳化硅的导热性，可满足汽车尾气碳烟颗粒过滤使用；
2、本发明中的碳化硅具有高温强度高、热震性好、导热性能高、高温下不收缩等优点，本发明采用粗细碳化硅为骨料，同时在碳化硅的表面包裹纳米铝溶胶液体、活性氧化铝、高岭土、微硅粉，利用纳米铝溶胶的高温活性，促进包裹在碳化硅表面的活性氧化铝、高岭土、微硅粉，在高温下原位生成莫来石，利用莫来石高温强度好、热震性好等优点，包覆在碳化硅颗粒间，使其形成碳化硅复合莫来石材质，同时添加造孔剂、石墨产生孔径、便于挤出，从而形成蜂窝陶瓷载体(DPF)；
3、本发明中所述的蜂窝陶瓷过滤器载体指标如下：碳化硅含量：85～90％、抗热震性：550度、孔径：8～20μm、孔隙率：≥45％、抗压强度：≥7MPa、碳烟颗粒捕获率：≥95％、使用温度：1500℃、荷重软化温度:1650℃。
附图说明
为了更清楚地说明本发明实施例或现有技术中的技术方案，下面将对实施例或现有技术描述中所需要使用的附图作简单地介绍，显而易见地，下面描述中的附图仅仅是本发明的一些实施例，对于本领域普通技术人员来讲，在不付出创造性劳动性的前提下，还可以根据这些附图获得其他的附图。
图1是实施例的产品指标图。
具体实施方式
下面结合附图对本发明作进一步的说明。
参看如图1所示，本具体实施方式(实施例一)采用的技术方案是：
1、按碳化硅粗粉A 60份、碳化硅微粉B 25份、活性ɑ-氧化铝微粉9份、高岭土5份、微硅粉2份、石墨1份，造孔剂10份、羟丙基甲基纤维素5份、硬脂酸盐1份、甘油2份、纯水25份配方称取各原料，然后将碳化硅粗粉A、碳化硅微粉B、活性ɑ-氧化铝微粉、高岭土、微硅粉、石墨、造孔剂原材料筛分，随后添加羟丙基甲基纤维素、硬脂酸盐，高速混合，得混合物；
2、在上述混合物中继续添加甘油、纳米铝溶胶、纯水，然后进行捏合、练泥、陈腐，再挤出成型，制成40*40mm、300目、壁厚为0.3mm的毛坯；
3、将上述毛坯进行微波干燥、切割、烧成，烧成温度为1500℃，然后进行保温，保温过程中，对每个测温点进行实时测温，单独调整，保证炉内不同位置温度控制在0～5℃以内，保温时间为4小时，还原气氛，即制得蜂窝陶瓷载体；
4、将40*40mm的蜂窝陶瓷载体进行双面交叉堵孔，使同一孔道的孔一面开口一面封闭，将40*40mm的多个蜂窝陶瓷载体进行拼接，拼接为160*160mm的载体，用外圆磨机加工成外径为144mm的圆形载体，在圆形载体表面进行植皮，植皮后进行二次烧结，烧成温度1200℃；其中，所采用的拼接料和植皮料一致，均由如下重量百分比成分组成：碳化硅80％、纤维棉10％％、氧化铝10％、羟丙基甲基纤维素2％。
进一步地，所述的步骤1中的碳化硅粗粉A的粒度为D50＝50μm，碳化硅微粉B粒度为D50＝11μm，活性ɑ-氧化铝微粉粒度为D50＝2μm，高岭土粒度为D50＝5μm，微硅粉粒度为D50＝1μm，石墨粒度为D50＝5μm，造孔剂为丙烯酸小球，粒度为50μm，羟丙基甲基纤维素为6000mpa.s。
进一步地，所述的步骤2中纳米铝溶胶粒径为10nm。
实施例二
本发明中碳化硅复合莫来石蜂窝陶瓷DPF载体的制备方法，包括如下步骤：
1、按碳化硅粗粉A 60份、碳化硅微粉B 30份、活性ɑ-氧化铝微粉6份、高岭土3.2份、微硅粉1.5份、石墨2份，造孔剂15份、羟丙基甲基纤维素8份、硬脂酸盐3份、甘油4份、纯水30份配方称取各原料，然后将碳化硅粗粉A、碳化硅微粉B、活性ɑ-氧化铝微粉、高岭土、微硅粉、石墨、造孔剂原材料筛分，随后添加羟丙基甲基纤维素、硬脂酸盐，高速混合，得混合物；
2、在上述混合物中继续添加甘油、纳米铝溶胶、纯水，然后进行捏合、练泥、陈腐，再挤出成型，制成40*40mm、300目、壁厚为0.25mm的毛坯；
3、将上述毛坯进行微波干燥、切割、烧成，烧成温度为1550℃，然后进行保温，保温过程中，对每个测温点进行实时测温，单独调整，保证炉内不同位置温度控制在0～5℃以内，保温时间为8小时，还原气氛，即制得蜂窝陶瓷载体；
4、将40*40mm的蜂窝陶瓷载体进行双面交叉堵孔，使同一孔道的孔一面开口一面封闭，将40*40mm的多个蜂窝陶瓷载体进行拼接，拼接为320*320mm的载体，用外圆磨机加工成外径为305mm的圆形载体，在圆形载体表面进行植皮，植皮后进行二次烧结，烧成温度1300℃；其中，所采用的拼接料和植皮料一致，均由如下重量百分比成分组成：碳化硅85％、纤维棉5％％、氧化铝10％、羟丙基甲基纤维素2％。
进一步地，所述的步骤1中的碳化硅粗粉A的粒度为D50＝40μm，碳化硅微粉B粒度为D50＝14μm，活性ɑ-氧化铝微粉粒度为D50＝2μm，高岭土粒度为D50＝3μm，微硅粉粒度为D50＝2μm，石墨粒度为D50＝3μm，造孔剂为活性炭颗粒，粒度为70μm，羟丙基甲基纤维素为6000mpa.s。
进一步地，所述的步骤2中纳米铝溶胶粒径为15nm。
以上所述，仅用以说明本发明的技术方案而非限制，本领域普通技术人员对本发明的技术方案所做的其它修改或者等同替换，只要不脱离本发明技术方案的精神和范围，均应涵盖在本发明的权利要求范围当中。

Claims (10)

1.一种蜂窝陶瓷过滤器载体，其特征在于：它由前驱体粉末和助剂组成，其中前驱体粉末与助剂的重量配比为85～90:10～15；其中，所述的前驱体粉末由如下重量份成分组成：碳化硅粗粉A40～70份、碳化硅微粉B15～30份、高岭土3～5份、活性ɑ-氧化铝微粉3～10份、硅微粉1～5份、石墨1～3份、造孔剂5～15份；所述的助剂由如下重量份成分组成：羟丙基甲基纤维素2～8份、硬脂酸盐1～4份、甘油2～6份、纳米铝溶胶液体5～15份、纯水25～30份。
2.根据权利要求1所述的一种蜂窝陶瓷过滤器载体，其特征在于：所述的碳化硅粗粉A为SIC≥98.5，粒径D50＝30～50μm，FeO含量≤0.1％。
3.根据权利要求1所述的一种蜂窝陶瓷过滤器载体，其特征在于：所述的碳化硅微粉B为SIC≥98.5,粒径D50＝10～14μm，FeO含量≤0.1％。
4.根据权利要求1所述的一种蜂窝陶瓷过滤器载体，其特征在于：所述的活性ɑ-氧化铝微粉的粒径D50＝1～2μm，Na2O含量≤0.1％。
5.根据权利要求1所述的一种蜂窝陶瓷过滤器载体，其特征在于：所述的高岭土的粒径D50＝1～4μm。
6.根据权利要求1所述的一种蜂窝陶瓷过滤器载体，其特征在于：所述的硅微粉的粒径D50＝1～3μm，SiO2≥99％。
7.根据权利要求1所述的一种蜂窝陶瓷过滤器载体，其特征在于：所述的石墨的粒径D50＝1～5μm。
8.根据权利要求1所述的一种蜂窝陶瓷过滤器载体，其特征在于：所述的造孔剂为有机丙烯酸小球、淀粉、活性炭中的一种,粒径D50＝30～80μm。
9.一种蜂窝陶瓷过滤器载体的制备方法，其特征在于：其操作步骤如下：
(1)、将碳化硅粗粉A、碳化硅微粉B、高岭土、活性ɑ-氧化铝微粉、硅微粉、石墨、造孔剂分别进行过筛处理，随后添加羟丙基甲基纤维素和硬脂酸盐，高速混合搅拌，得混合物；
(2)、向上述混合物中继续添加甘油、纳米铝溶胶液体和纯水，然后进行捏合、练泥、陈腐，最后挤出成型，形成毛坯；
(3)、将上述毛坯进行微波干燥、切割、烧成，烧成温度为1500-1600℃，再进行保温，保温过程中，对每个测温点进行实时测温，单独调整，保证炉内不同位置温度控制在0～5℃以内，保温时间为4-10小时，还原气氛，即制得蜂窝陶瓷载体；
(4)、将上述蜂窝陶瓷载体进行双面交叉堵孔、使同一孔道的孔一面开口一面封闭，再将多个蜂窝陶瓷载体进行拼接，构成一个新的载体，用外圆磨机加工成圆形载体，在圆形载体表面进行植皮，植皮后进行二次烧结，烧成温度1200-1300℃。
10.根据权利要求9所述的一种蜂窝陶瓷过滤器载体的制备方法，其特征在于：所述的步骤(4)中拼接所采用的拼接料和植皮所采用的植皮料一致，均由如下质量百分比成分组成：碳化硅80-90％、纤维棉5-10％％、氧化铝10％、羟丙基甲基纤维素2％。
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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111299547A (zh) * 2020-03-18 2020-06-19 安徽华德电力技术工程有限公司 一种耐高温复合材料及其制备方法和应用
CN114524675A (zh) * 2022-02-22 2022-05-24 山东奥福环保科技股份有限公司 一种硅结合碳化硅质柴油颗粒过滤器及其制备方法
CN115536427A (zh) * 2022-10-21 2022-12-30 昆明理工大学 一种碳化硅基固液气分离用多孔陶瓷材料及其制备方法

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111299547A (zh) * 2020-03-18 2020-06-19 安徽华德电力技术工程有限公司 一种耐高温复合材料及其制备方法和应用
CN114524675A (zh) * 2022-02-22 2022-05-24 山东奥福环保科技股份有限公司 一种硅结合碳化硅质柴油颗粒过滤器及其制备方法
CN115536427A (zh) * 2022-10-21 2022-12-30 昆明理工大学 一种碳化硅基固液气分离用多孔陶瓷材料及其制备方法

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