CN115073135B - 一种大规格高承压薄壁堇青石蜂窝陶瓷载体的制备方法 - Google Patents

一种大规格高承压薄壁堇青石蜂窝陶瓷载体的制备方法 Download PDF

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CN115073135B
CN115073135B CN202210886637.XA CN202210886637A CN115073135B CN 115073135 B CN115073135 B CN 115073135B CN 202210886637 A CN202210886637 A CN 202210886637A CN 115073135 B CN115073135 B CN 115073135B
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史亮
冯家迪
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JIANGSU PROVINCE YIXING NONMETALLIC CHEMICAL MACHINERY FACTORY CO Ltd
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Abstract

本发明公开了一种大规格高承压薄壁堇青石蜂窝陶瓷载体的制备方法,制备原料由以下重量百分比的各组分组成:滑石25‑42%,非活性氧化铝5‑10%,二氧化硅12‑16%,高岭土20‑30%,活性氧化铝5‑10%,表面活性剂0.2‑0.5%,粘结剂2‑6%,润滑剂1‑3%,各组分之和为100%。本发明采用特定的原料种类和规格、配合合理的用量,结合改进的制备工艺,能够制备出直径≥177mm,壁厚4mil的大规格薄壁堇青石蜂窝陶瓷载体,产品薄壁开裂率低于5%,成品率高;此外产品还具有很好的力学性能,其中,A向抗压强度不低于12MPa,B向抗压强度不低于4MPa,C向抗压强度不低于0.3MPa。

Description

一种大规格高承压薄壁堇青石蜂窝陶瓷载体的制备方法
技术领域
本发明涉及蜂窝陶瓷载体制备技术领域,尤其是涉及一种大规格高承压薄壁堇青石蜂窝陶瓷载体的制备方法。
背景技术
柴油机尾气净化用大规格堇青石蜂窝陶瓷载体,直径一般>177mm,载体采用蜂窝形状结构,包含孔道壁隔开的许多独立孔道,孔道密度在280个以上/英寸2,常规孔道壁厚≥0.17mm,而对于薄壁产品,其壁厚一般是是mil级别。
现有的薄壁堇青石蜂窝陶瓷载体大多采用堇青石原位合成,所采用的原料包括滑石、氧化铝、二氧化硅、高岭土以及添加剂等组分,由于物料各自的物理、化学特性不同,使得在产品的制备过程中会产生薄壁开裂,从而产生缺陷,同时由于壁薄,也会使得产品的耐压能力所有降低,进而影响柴油机尾气净化的效果。
发明内容
针对现有技术存在的上述问题,本申请所要解决的技术问题是提供一种大规格高承压薄壁堇青石蜂窝陶瓷载体的制备方法,减少薄壁开裂并有效提高产品的耐压能力,能满足柴油车国六排放标准的使用需求。
为了解决上述技术问题,本发明的技术方案如下:
一种大规格高承压薄壁堇青石蜂窝陶瓷载体的制备方法,制备原料由以下重量百分比的各组分组成:滑石25-42%,非活性氧化铝5-10%,二氧化硅12-16%,高岭土20-30%,活性氧化铝5-10%,表面活性剂0.2-0.5%,粘结剂2-6%,润滑剂1-3%,各组分之和为100%;具体步骤如下:
1)先将滑石、非活性氧化铝、高岭土、活性氧化铝、二氧化硅、粘结剂进行混合,然后加入表面活性剂继续混合,最后再与润滑剂进行混合;
2)在练泥机中充分练泥;
3)在成型机中一次成型,控温不超过38℃;
4)窑炉煅烧,按照15~30℃/h进行程序升温至1400±20℃,保温不低于8h;
5)精磨尺寸加工,植皮,获得成品;
其中,大规格为直径>177mm,薄壁为壁厚4mil,高承压为A向抗压强度不低于12MPa,B向抗压强度不低于4MPa,C向抗压强度不低于0.3MPa。
所述的大规格高承压薄壁堇青石蜂窝陶瓷载体的制备方法,滑石的粒径范围为6-14μm;滑石中MgO重量占比>30%,且滑石中CaO、K2O和Na2O重量之和占比<0.5%。
所述的大规格高承压薄壁堇青石蜂窝陶瓷载体的制备方法,非活性氧化铝的粒径范围为2-8μm,纯度>99%。
所述的大规格高承压薄壁堇青石蜂窝陶瓷载体的制备方法,二氧化硅的粒径范围为2-8μm,纯度>99%。
所述的大规格高承压薄壁堇青石蜂窝陶瓷载体的制备方法,高岭土的粒径范围为1-5μm,高岭土中Al2O3重量占比>35%,SiO2重量占比>45%。
所述的大规格高承压薄壁堇青石蜂窝陶瓷载体的制备方法,活性氧化铝中,Al2O3重量占比>65%,CaO+K2O+Na2O重量占比<0.5%,活性氧化铝的比表面积150~350m2/g。
所述的大规格高承压薄壁堇青石蜂窝陶瓷载体的制备方法,步骤4)中,按照15~20℃/h进行程序升温至1400±20℃,保温8-10h。
有益效果:与现有技术相比,本发明的技术优势在于:
1)本发明采用特定的原料种类和规格、配合合理的用量,结合改进的制备工艺,能够制备出直径≥177mm,壁厚4mil的大规格薄壁堇青石蜂窝陶瓷载体,产品薄壁开裂率低于5%,成品率高。
2)本申请在成品率高的基础上,还能确保产品具有很好的力学性能,其中,A向抗压强度不低于12MPa,产品薄壁开裂率少于5%,成品率非常高,能满足使用需求。
附图说明
图1是大规格高承压薄壁蜂窝陶瓷载体的薄壁结构扫描电镜图。
具体实施方式
下面结合实施例对本发明进行具体描述。
以下实施例中所使用的原料要求如表1所示。
表1原料规格表
Figure BDA0003766049830000031
实施例1
按照表2的原料用量制备大规格高承压薄壁蜂窝陶瓷载体,其中,大规格为直径>177mm,典型的尺寸包括330mm,305mm,267mm,228mm,190mm,177.8mm;薄壁为壁厚4mil。本实施例制备的产品(圆柱形产品)的直径为330mm,薄壁为壁厚4mil。
具体的制备步骤如下:
1)先将滑石、非活性氧化铝、高岭土、活性氧化铝、二氧化硅、粘结剂进行混合,然后加入表面活性剂继续混合,最后再与润滑剂进行混合;
2)在练泥机中充分练泥;
3)在成型机中一次成型,控温不超过38℃(超过38℃无法成型);
3)窑炉煅烧,按照20℃/h进行程序升温至1400±20℃,保温不低于8h。
4)精磨尺寸加工,植皮(常规方法,可参照CN105777194A进行),获得成品。
表2产品组分和用量(单位为份数)以及检测结果
Figure BDA0003766049830000032
Figure BDA0003766049830000041
表2中,表面活性剂可以为妥尔油、月桂酸、丙烯酸乳液,本次产品制备选择丙烯酸乳液(深圳市吉田化工有限公司,固含量44%)。粘结剂为甲基纤维素(市售,泸州4000)。润滑剂可以为皂液或聚α烯烃,本次使用聚α烯烃(市售,型号为PAO2、PAO3、PAO4)。非活性氧化铝即为常规市售的氧化铝产品。薄壁开裂直接目测检测。
抗压强度检测采用国家标准(GB/T 25994-2010)进行检测,产品为圆形,施加负荷的速率为1.5MPa/s,单位为MPa。
采用压汞法测试孔隙度(GB/T 21650.1-2008/ISO 15901-1:2005),测试参数设置为:汞接触角为130°;汞表面张力0.485N·m-1;汞密度(20℃)13.5335g/mL;使用步进模式采集压力数据,压力平衡时间为10s;无预处理。
从表2可知,原料的规格、产品的特定组分及其合理的用量,是决定产品是否开裂以及产品强度的主要因素之一,与其他产品相比,本实施例中的产品3和产品4效果最为突出。
实施例2
按照实施例1的方法制备产品3不同在于,在步骤3)中,窑炉煅烧,程序升温至200-600℃时,分别按照15℃/h,20℃/h,25℃/h进行程序升温至1400±20℃,保温不低于6-20h。对产品的开裂数进行检测,结果如表3所示。
表3产品检测结果
Figure BDA0003766049830000051
从表3可以看出,在产品组成固定的情况下,在200-600℃范围,控制升温速率,有利于提高产品的合格率。而合理的保温时间是确保产品强度以及孔隙度等其他性能参数的主要依据,并应重点考虑合理的生产能耗。

Claims (1)

1.一种大规格高承压薄壁堇青石蜂窝陶瓷载体的制备方法,其特征在于,制备原料由以下重量百分比的各组分组成:滑石25-42%,非活性氧化铝5-10%,二氧化硅12-16%,高岭土20-30%,活性氧化铝5-10%,表面活性剂0.2-0.5%,粘结剂2-6%,润滑剂1-3%,各组分之和为100%;具体步骤如下:
1)先将滑石、非活性氧化铝、高岭土、活性氧化铝、二氧化硅、粘结剂进行混合,然后加入表面活性剂继续混合,最后再与润滑剂进行混合;
2)在练泥机中充分练泥;
3)在成型机中一次成型,控温不超过38℃;
4)窑炉煅烧,按照15~20℃/h进行程序升温至1400±20℃,保温8-10h;
5)精磨尺寸加工,植皮,获得成品;
其中,大规格为直径>177mm,薄壁为壁厚4mil,高承压为A向抗压强度不低于12MPa,B向抗压强度不低于4MPa,C向抗压强度不低于0.3MPa;
滑石的粒径范围为6-14μm,滑石中MgO重量占比>30%,且滑石中CaO、K2O和Na2O重量之和占比<0.5%;非活性氧化铝的粒径范围为2-8μm,纯度>99%;二氧化硅的粒径范围为2-8μm,纯度>99%;高岭土的粒径范围为1-5μm,高岭土中Al2O3重量占比>35%,SiO2重量占比>45%;活性氧化铝中,Al2O3重量占比>65%,CaO+K2O+Na2O重量占比<0.5%,活性氧化铝的比表面积150~350m2/g。
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