CN116063095A - 薄壁、大中值孔径堇青石蜂窝陶瓷过滤器及其制备方法和应用 - Google Patents

薄壁、大中值孔径堇青石蜂窝陶瓷过滤器及其制备方法和应用 Download PDF

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CN116063095A
CN116063095A CN202310200956.5A CN202310200956A CN116063095A CN 116063095 A CN116063095 A CN 116063095A CN 202310200956 A CN202310200956 A CN 202310200956A CN 116063095 A CN116063095 A CN 116063095A
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honeycomb ceramic
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程国园
潘吉庆
黄妃慧
刘洪月
江涛
张兆合
刘坤
关洋
陈一韬
邢延岭
郝立苗
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Shandong Aofu Environmental Protection Science & Technology Co ltd
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Abstract

本发明属于堇青石蜂窝陶瓷过滤器技术领域，具体涉及一种薄壁、大中值孔径堇青石蜂窝陶瓷过滤器及其制备方法和应用。该方法包括以下步骤：1）采用干法将各原材料混合均匀；2）先将高岭土、氧化铝、滑石、二氧化硅、造孔剂和粘结剂混合均匀，再将混合均匀的粉料与润滑剂、水湿混捏合并练制成具有塑性的泥段；3）挤出成蜂窝状结构并干燥定型；4）烧成：室温‑500℃以小于30℃/h的速率升温，500‑1000℃以小于40℃/h的速率升温，1000℃‑保温温度以小于70℃/h的速率升温，保温时间8~16小时；5）打孔、堵孔、围边，得到成品。本发明可以制备得到壁厚6mil~8mil，中值孔径10~16μm、D10≥6.5μm、D90≤28μm微孔分布、45~55%孔隙率的过滤器。

Description

薄壁、大中值孔径堇青石蜂窝陶瓷过滤器及其制备方法和应用
技术领域
本发明属于堇青石蜂窝陶瓷过滤器技术领域，具体涉及一种薄壁、大中值孔径堇青石蜂窝陶瓷过滤器及其制备方法和应用。
背景技术
汽车尾气排气颗粒，尤其是微细粒子以及有致癌突变作用的多环芳烃，会对环境和人体健康造成极大危害。随着环境污染的日益严重，汽车尾气排放的控制也越来越严苛，蜂窝陶瓷过滤器因其独特的壁流式结构在去除汽车尾气颗粒物方面得到广泛应用，尤其在柴油发动机和一些汽油直喷发动机情况下，可以很好的过滤掉尾气中的碳烟颗粒，净化排放尾气。但是，随着排放法规的不断加严，传统的后处理技术难以满足其要求，必须对其进行优化升级，开发满足更严苛法规限制的蜂窝陶瓷新技术，因此薄壁蜂窝陶瓷过滤器应运而生。
目前满足国六及市场法规限值标准并且大量应用的颗粒过滤器壁厚一般超过8mil，但是世界各地法规及执行标准存在差异，客户需求也存在多元化，随着法规的升级，后处理***压降的降低成为了关键技术难题之一。在载体方面，一方面能够通过载体壁厚的薄壁化降低压降，另一方面通过增大过滤器的中值孔径、缩窄微孔分布也能达到降低压降的目的。因此，为了满足不同地区市场需求，公司开发6mil~8mil薄壁、10~16μm中值孔径、D10≥6.5μm、D90≤28μm窄微孔分布、45~55%孔隙率的过滤器产品。其中，过滤器壁厚的薄壁化对原材料设置了限制条件，是由于蜂窝陶瓷使用模具挤制成型，模具槽宽越窄允许通过的原材料粒度越细，挤制的产品壁厚越薄，另外，原材料之间的架桥效应对原材料的粒度进行了更严格的限制，为了消除架桥效应，原材料粒度需要进一步细化。但是，产品中值孔径越大需要的原材料粒度越粗，因此薄壁和大中值孔径这两个特性是一对矛盾点，也是本发明所要解决的难点。在薄壁的限制条件下，本发明所要解决的另外一个难点是45~55%的低孔隙率实现10~16μm的中值孔径，因为通过提高过滤器的孔隙率也能够达到增大中值孔径的目的，比如国六汽油颗粒过滤器60~65%的孔隙率也能够实现10~16μm的中值孔径，因此45~55%低孔隙率增加了大中值孔径的技术难度。
发明内容
为解决现有技术的不足，本发明提供了一种薄壁、大中值孔径堇青石蜂窝陶瓷过滤器及其制备方法和应用。本发明突破了薄壁、大中值孔径、窄孔分布过滤器开发的技术难点，即薄壁和大中值孔径这两个特性之间的矛盾的技术难点，以及低孔隙率增加了大中值孔径的技术难点，开发了壁厚6mil~8mil、中值孔径10~16μm、D10≥6.5μm、D90≤28μm微孔分布、45~55%孔隙率的过滤器，满足了不同地区市场的多元化需求，助力了大气污染治理。
本发明所提供的技术方案如下：
一种薄壁、大中值孔径堇青石蜂窝陶瓷过滤器的制备方法，包括以下步骤：
1）采用干法将制备堇青石用的各原材料混合均匀；
2）先将生高岭土、煅烧高岭土、氧化铝、滑石、二氧化硅、造孔剂和粘结剂混合均匀，再将混合均匀的粉料与润滑剂、水湿混捏合并练制成具有塑性的泥段；
3）将塑性泥段挤出成蜂窝状结构并干燥定型；
4）对生坯体进行烧成：室温-500℃以小于30℃/h的速率升温，500-1000℃以小于40℃/h的速率升温，1000℃-保温温度以小于70℃/h的速率升温，保温时间8~16小时，得到堇青石蜂窝陶瓷体，保温温度为1410到1440℃；
5）将得到的堇青石蜂窝陶瓷体进行打孔、堵孔、围边，得到成品薄壁、大中值孔径堇青石蜂窝陶瓷过滤器。
基于上述技术方案，可以制备得到壁厚6mil~8mil，中值孔径10~16μm、D10≥6.5μm、D90≤28μm微孔分布、45~55%孔隙率的过滤器。
具体的，滑石的粒度D50为40~44μm，D100≤100μm；添加量≤45wt%。
上述技术方案中，滑石的粒度分布过大，会导致挤出成型困难、产品微孔分布宽。
具体的，生高岭土的粒度D50为8~10μm，D100≤21μm；添加量≤15wt%。
上述技术方案中，生高岭土的粒度分布过大，会导致产品微孔分布宽。
具体的，煅烧高岭土的粒度D50为8~10μm，D100≤21μm；添加量≤15wt%。
上述技术方案中，煅烧高岭土的粒度分布过大，会导致产品微孔分布宽。
具体的，氧化铝的粒度D50为8~10μm，D100≤22μm；添加量≤21wt%。
上述技术方案中，氧化铝的粒度分布过大，会导致产品微孔分布宽。
具体的，二氧化硅的粒度D50为28~30μm，D100≤63μm；添加量≤23wt%。
上述技术方案中，二氧化硅的粒度分布过大，会导致挤出成型困难、产品微孔分布宽。
具体的，造孔剂的粒度D50为36~39μm，D100≤80μm；添加量≤30wt%。
上述技术方案中，造孔剂的粒度分布过大，会导致挤出成型困难、产品微孔分布宽。
具体的，粘结剂的添加量≤10wt%。
具体的，润滑剂的添加量≤4wt%。
本发明还提供了根据上述制备方法制备得到的薄壁、大中值孔径堇青石蜂窝陶瓷过滤器。
本发明对蜂窝结构体中蜂窝格子的形状没有特别限制，可以采用三角形、四角形、六角形等单一孔形，也可以是四角形、六角形、非对称形等多种孔型，在蜂窝结构体中没有必要采用单一孔形状，优选采用例如四角形孔。
本发明对蜂窝结构的孔密度没有特别限制，可以是200cpsi、300cpsi、400cpsi等一切能够挤制成蜂窝形状的孔密度，实施例仅仅是为清楚地说明所作的举例，而并非对实施方式的限定。
本发明可以作为柴油颗粒过滤器，也可以作为汽油颗粒过滤器。
本发明涉及一种堇青石蜂窝陶瓷过滤器及其制备方法，尤其涉及一种薄壁、大中值孔径、窄孔分布、低孔隙率蜂窝陶瓷过滤器及其制备方法。本发明克服了薄壁、低孔隙率和大中值孔径这些矛盾点，开发了薄壁、低孔隙率、大中值孔径、窄微孔分布的蜂窝陶瓷过滤器，弥补了市场缺失，为市场的多元化需求提供了保障。
附图说明
图1是本发明实施例5的蜂窝陶瓷过滤器微孔分布。
具体实施方式
以下对本发明的原理和特征进行描述，所举实施例只用于解释本发明，并非用于限定本发明的范围。
制备薄壁、大中值孔径堇青石蜂窝陶瓷的原材料如表1所示。
表1 原材料列表
薄壁、大中值孔径堇青石蜂窝陶瓷过滤器的制备方法，包括以下步骤：
1）采用干法将制备堇青石用的各原材料混合均匀；
2）先将生高岭土、煅烧高岭土、氧化铝、滑石、二氧化硅、造孔剂和粘结剂混合均匀，再将混合均匀的粉料与润滑剂、水湿混捏合并练制成具有塑性的泥段；
3）将塑性泥段挤出成蜂窝状结构并干燥定型；
4）对生坯体进行烧成，具体参数统一为：室温-500℃以约10℃/h的速率升温，500-1000℃以约20℃/h的速率升温，1000℃-1430℃以约25℃/h的速率升温，保温时间10小时，得到堇青石蜂窝陶瓷体；
5）将得到的堇青石蜂窝陶瓷体进行打孔、堵孔、围边，得到成品薄壁、大中值孔径堇青石蜂窝陶瓷过滤器。
具体实施方式如表2所示：
表2 实施方式列表
表2中各成分的含量按照wt%计入。
比较例1、比较例2是使用与表1中列举原材料的D50相同、D100超出控制范围的粒度分布宽的普通原材料制备的蜂窝陶瓷过滤器，实施例1~6是使用表1中粒度分布窄的原材料制备的薄壁、大中值孔径堇青石蜂窝陶瓷过滤器。表1中原材料粒度分布较窄，能够满足薄壁6~8mil挤出成型性能，而比较例1、比较例2中未对原材料粒度D100进行限制，可能会出现6~8mil薄壁蜂窝陶瓷过滤器挤制成型困难的现象，蜂窝陶瓷的微孔分布宽。同时，粒度分布窄的原材料制备的蜂窝陶瓷过滤器微孔分布非常窄，因此相同粒度D50的原材料，原材料粒度分布越窄，产品微孔分布越窄，微孔越均匀、连通性越好，产品的过滤效率越高。
对比实施例1~6、比较例1~2可以看出，通过调整原材料种类、配比、粒度分布、可以调整蜂窝陶瓷的孔隙率、微孔分布等特性，而孔隙率的调整不仅仅能够通过原材料种类、配比来达到，通过调整造孔剂添加量也可以达到调整孔隙率的目的，这里有限的实施例中未进行列举。
薄壁产品对泥料的料性要求非常高，生高岭土的加入对薄壁产品的挤制成型是非常有利的，同时，生高岭土能够增强坯体强度。
以上所述仅为本发明的较佳实施例，并不用以限制本发明，凡在本发明的精神和原则之内，所作的任何修改、等同替换、改进等，均应包含在本发明的保护范围之内。

Claims (10)

1.一种薄壁、大中值孔径堇青石蜂窝陶瓷过滤器的制备方法，其特征在于，包括以下步骤：
1）采用干法将制备堇青石用的各原材料混合均匀；
2）先将生高岭土、煅烧高岭土、氧化铝、滑石、二氧化硅、造孔剂和粘结剂混合均匀，再将混合均匀的粉料与润滑剂、水湿混捏合并练制成具有塑性的泥段；
3）将塑性泥段挤出成蜂窝状结构并干燥定型；
4）对生坯体进行烧成：室温-500℃以小于30℃/h的速率升温，500-1000℃以小于40℃/h的速率升温，1000℃-保温温度以小于70℃/h的速率升温，保温时间8~16小时，得到堇青石蜂窝陶瓷体，保温温度为1410到1440℃；
5）将得到的堇青石蜂窝陶瓷体进行打孔、堵孔、围边，得到成品薄壁、大中值孔径堇青石蜂窝陶瓷过滤器。
2.根据权利要求1所述的薄壁、大中值孔径堇青石蜂窝陶瓷过滤器的制备方法，其特征在于：滑石的粒度D50为40~44μm，D100≤100μm；添加量≤45wt%。
3.根据权利要求1所述的薄壁、大中值孔径堇青石蜂窝陶瓷过滤器的制备方法，其特征在于：生高岭土的粒度D50为8~10μm，D100≤21μm；添加量≤15wt%。
4.根据权利要求1所述的薄壁、大中值孔径堇青石蜂窝陶瓷过滤器的制备方法，其特征在于：煅烧高岭土的粒度D50为8~10μm，D100≤21μm；添加量≤15wt%。
5.根据权利要求1所述的薄壁、大中值孔径堇青石蜂窝陶瓷过滤器的制备方法，其特征在于：氧化铝的粒度D50为8~10μm，D100≤22μm；添加量≤21wt%。
6.根据权利要求1所述的薄壁、大中值孔径堇青石蜂窝陶瓷过滤器的制备方法，其特征在于：二氧化硅的粒度D50为28~30μm，D100≤63μm；添加量≤23wt%。
7.根据权利要求1所述的薄壁、大中值孔径堇青石蜂窝陶瓷过滤器的制备方法，其特征在于：造孔剂的粒度D50为36~39μm，D100≤80μm；添加量≤30wt%。
8.一种根据权利要求1至7任一所述的制备方法制备得到的薄壁、大中值孔径堇青石蜂窝陶瓷过滤器。
9.根据权利要求8所述的薄壁、大中值孔径堇青石蜂窝陶瓷过滤器，其特征在于：
蜂窝结构体中蜂窝格子的形状选自三角形、四角形或六角形孔形中的任意一种或多种；
蜂窝结构的孔密度的选择包括但不限于：200cpsi、300cpsi和400cpsi。
10.一种根据权利要求8或9所述的薄壁、大中值孔径堇青石蜂窝陶瓷过滤器的应用，其特征在于：作为柴油颗粒过滤器或汽油颗粒过滤器。
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