CN112552071B - 一种SiC质柴油车颗粒捕集器及其制备方法 - Google Patents
一种SiC质柴油车颗粒捕集器及其制备方法 Download PDFInfo
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Abstract
本发明公开了一种SiC质柴油车颗粒捕集器,首先将萜烯树脂、松节油、柴油、邻苯二甲酸二乙酯进行剪切处理制备成型剂,然后以SiC粉末、金属硅粉和成型剂为原料进行混料、干燥、挤压成型和控制烧结而成。本发明所得SiC质柴油车颗粒捕集器具有强度高、化学及热稳定性好,易于成型,尤其可实现超薄壁厚等优点,具有重要的推广应用价值。
Description
技术领域
本发明属于材料科学与工程技术领域,具体涉及一种SiC质柴油车颗粒捕集器的及其制备方法。
背景技术
空气中的细颗粒物(PM2.5)是导致雾霾天气的最主要因素,而柴油车尾气是PM2.5的主要来源之一。柴油车尾气中PM的排放量比汽油车高30~60倍,且PM直径大多在0.1~10μm之间,表面具有易挥发和可溶的致癌物,易被人类吸收进入肺部并沉积下来,严重威胁人类生活健康。
为了降低柴油车排放水平,改善空气质量,我国实施了日益严格的柴油车排放标准。目前,最常用且有效的降低柴油车尾气颗粒物排放技术是柴油车颗粒捕集器(DieselParticulate Filter,简称DPF)。DPF安装在排气管的后侧,当尾气通过DPF,PM会被DPF中过滤体截留,从而降低PM的排放。为了提高DPF的过滤效率,通常会将DPF制作成蜂窝管状,并将蜂窝管状中相邻的通道两端进行交替堵孔得到壁流式蜂窝陶瓷过滤体。由于DPF体积的限制,壁流式蜂窝陶瓷过滤体的过滤面积受到限制,在单位体积下,仅能通过降低壁流式蜂窝陶粒过滤体壁厚的方式,进一步提升过滤效率,以满足日益严苛的柴油车排放标准。
目前,DPF多采用陶瓷基作为过滤基体,包括堇青石质和碳化硅(SiC)质等,其中SiC质DPF具有优异的耐热、耐蚀性能和导热性能,机械强度大,能够承受恶劣的工况,耐久性好等特点,是未来的发展趋势。但是SiC质DPF在制备过程中,由于SiC粉体与水的亲水性差,虽然通过加入纤维素醚、表面活性剂等常规技术可以改善SiC泥料的可塑性,但是,面对DPF对于超薄壁厚的需求,现有技术难以满足要求。因此,进一步探索和研究具有强度高、化学及热稳定性好、易于成型、可实现超薄壁厚等优点的SiC质柴油车颗粒捕集器并优化其制备工艺,对大气污染防治,提升人民生活品质具有重大的意义。
发明内容
本发明的主要目的在于针对现有技术存在的不足,提供一种SiC质柴油车颗粒捕集器,它具有强度高、化学及热稳定性好,易于成型,可实现超薄壁厚等优点。
为实现上述目的,本发明采用的技术方案为:
一种SiC质柴油车颗粒捕集器,首先将萜烯树脂、松节油、柴油、邻苯二甲酸二乙酯进行剪切处理制备成型剂,然后以SiC粉末、金属硅粉和成型剂为原料进行混料、干燥、挤压成型和控制烧结而成。
上述方案中,所述SiC粉末、金属硅和成型剂的质量比为100:(5~10):(10~15)。
上述方案中,所述萜烯树脂、松节油、柴油、邻苯二甲酸二乙酯的质量比为100:(50~70):(20~40):(2~3)。
上述一种SiC质柴油车颗粒捕集器的制备方法,具体包括如下步骤:
1)烧制原料制备
将萜烯树脂、松节油、柴油、邻苯二甲酸二乙酯按比例混合,进行剪切处理,得成型剂;然后将SiC粉末、金属硅粉和成型剂搅拌混合均匀,干燥,得烧制原料;
2)素胚成型
将所得烧制原料进行挤出成型得到所需形状的试件,再进行鼓风干燥,得成型后的素胚;
3)烧制
将所得素胚在真空或惰性气氛条件下,首先以6-10℃/min的速率升温至800~900℃,保温2~4h,再以10-15℃/min的速率升温至2080~2150℃,保温1~1.5h,随炉冷却至室温,即得所述SiC质柴油车颗粒捕集器。
上述方案中,所述萜烯树脂、松节油、柴油、邻苯二甲酸二乙酯的质量比为100:(50~70):(20~40):(2~3)。
上述方案中,所述剪切处理温度为105~120℃条件下,剪切速率为200~300r/min,时间为20-25min。
上述方案中,所述SiC粉末、金属硅和成型剂的质量比100:(5~10):(10~15)。
上述方案中,所述鼓风干燥温度为60~80℃,时间为12~24h。
上述方案中,所述萜烯树脂的软化点为90~100℃;所述松节油的蒎烯含量大于80%,酸值小于1mg/g。
上述方案中,所述柴油为5#、0#或者-10#柴油;所述邻苯二甲酸二乙酯的纯度大于98%。
上述方案中,所述SiC粉末的平均粒度为5~40μm,纯度大于97%;所述金属硅粉平均粒径<80μm,硅含量>95%。
根据上述方案所得SiC质柴油车颗粒捕集器,过滤器通道壁厚0.2~0.3mm,开孔率>47%,抗压强度>20MPa,热膨胀系数≤1.8×10-6℃-1。
本发明通过对成型剂进行设计和优化,可极大地改善SiC的可塑性,使SiC质柴油车颗粒捕集器在成型过程中,在保证体积稳定性的前提下,能够获得更薄的壁厚,从而提高柴油车颗粒捕集器单位体积下的过滤面积,并降低过滤过程中的排气背压。在此基础上,设计与材料组成相匹配的干燥和烧结工艺制度,制得具有超薄壁厚、强度高和热膨胀系数低的SiC质柴油车颗粒捕集器,具体为:
本发明首先利用萜烯树脂、松节油、柴油和邻苯二甲酸二乙酯进行剪切复合得到具有流动性好、粘结性能高、干燥挥发速度适中的成型剂,能够在常温下将SiC和金属硅粉等较好的粘接在一起,且具有优异的可塑性;其中松节油和柴油的饱和蒸气压分别为2.7kPa和4.0kPa,在素胚干燥过程中,两者相互作用下可实现缓慢挥发,使所得成型剂中的溶剂组分以适宜的释放速度,既可有效防止素胚的干燥开裂,又能在较短的时间内使素胚内残留少;待松节油和柴油释放完全后,萜烯树脂和邻苯二甲酸二乙酯能够将SiC和金属硅粉良好的粘接在一起,兼顾强度和韧性,使素胚在烧结过程中具有良好的体积稳定性。
在干燥和烧结工艺方面,本发明首先采用60~80℃低温干燥,可以有效防止素胚干燥收缩开裂;然后先升温至800~900℃,使萜烯树脂、邻苯二甲酸二乙酯以及少量掺量的松节油和柴油碳化(以上物质均由含有C、H、O的高分子物质组成,在高温烧结过程中,会碳化,生产碳和气体),碳化生成的气体排出也进一步提高了产品的开孔率,最后升温至2080~2150℃,一方面是原料中的SiC颗粒之间开始烧结,另一方面使碳化产生的碳和金属硅粉反应,产生活性高的SiC晶体,这些初生晶体具有较高的活性,能够将原料中的SiC颗粒进一步粘接,由于碳和金属硅粉有效反应了,最终产品中得到的SiC纯度高,具有更为优异的产品品质。
与现有技术相比,本发明的有益效果为:
本发明通过配方设计提升SiC泥料的可塑性,辅以相匹配的烧结工艺,所得SiC质柴油车颗粒捕集器具有强度高、化学及热稳定性好,易于成型,尤其可实现超薄壁厚(0.3mm以下)结构的制备,具有重要的推广应用价值。
具体实施方式
为使本领域普通技术人员充分理解本发明的技术方案和有益效果,以下结合具体实施例进行进一步说明。
以下实施例中,采用的SiC粉末的平均粒度为20μm,纯度为98wt%;金属硅粉平均粒径为25μm,硅含量为96wt%。
采用的萜烯树脂的软化点为90~100℃;所述松节油的蒎烯含量大于80%,酸值小于1mg/g。
采用的柴油为0#柴油。
实施例1
一种SiC质柴油车颗粒捕集器,其制备方法包括如下步骤:
1)烧制原料制备
将萜烯树脂、松节油、柴油、邻苯二甲酸二乙酯按100:50:20:2的质量比称料,在105℃条件下,利用高速剪切机分散混合,控制剪切速率为200r/min,时间为20min;得到成型剂;
将SiC粉末、金属硅粉、成型剂按100:5:10的质量比称料,通过搅拌机搅拌3min,再放入常温干燥箱中保存,制得SiC质柴油车颗粒捕集器烧制原料;
2)素胚成型
将步骤1)所得烧制原料,采用挤出成型机制成所需形状的试件,再放入60℃的鼓风干燥箱中干燥12h,制得SiC质柴油车颗粒捕集器素胚;
3)烧制
将步骤2)所得素胚放入高温炉中,抽真空或充入惰性气体,首先以6℃/min的速度升温至800℃,保温2h,再以10℃/min的速度升温至2080℃,保温1h,随炉冷却至室温,制得SiC质柴油车颗粒捕集器。
经测试,本实施例所得SiC质柴油车颗粒捕集器,过滤器通道壁厚0.23mm,开孔率50%,抗压强度25Mpa(边长为26mm的立方体试样;下同),热膨胀系数1.7×10-6℃-1。
实施例2
一种SiC质柴油车颗粒捕集器,其制备方法包括如下步骤:
1)烧制原料制备
将萜烯树脂、松节油、柴油、邻苯二甲酸二乙酯按100:70:40:3的质量比称料,在120℃条件下,利用高速剪切机分散混合,剪切速率为300r/min,时间为25min,得到成型剂;
将SiC粉末、金属硅粉、成型剂按100:10:15的质量比称料,通过搅拌机搅拌6min,再放入常温干燥箱中保存,制得SiC质柴油车颗粒捕集器烧制原料;
2)素胚成型
将步骤1)所得烧制原料,采用挤出成型机制成所需形状的试件,再放入80℃的鼓风干燥箱中干燥24h,制得SiC质柴油车颗粒捕集器素胚;
3)烧制
将步骤2)所得素胚放入高温炉中,抽真空或充入惰性气体,首先以10℃/min的速度升温至900℃,保温4h,再以15℃/min的速度升温至2150℃,保温1.5h,完成后随炉冷却至室温,制得SiC质柴油车颗粒捕集器。
经测试,本实施例所得SiC质柴油车颗粒捕集器,过滤器通道壁厚0.25mm,开孔率51%,抗压强度28MPa,热膨胀系数1.6×10-6℃-1。
实施例3
一种SiC质柴油车颗粒捕集器,其制备方法包括如下步骤:
1)烧制原料制备
将萜烯树脂、松节油、柴油、邻苯二甲酸二乙酯按100:60:30:3的质量比称料,在110℃条件下,利用高速剪切机分散混合,控制剪切速率为240r/min,时间为25min,得到成型剂;
将SiC粉末、金属硅粉、成型剂按100:8:13的质量比称料,通过搅拌机搅拌5min,再放入常温干燥箱中保存,制得SiC质柴油车颗粒捕集器烧制原料;
2)素胚成型
将步骤1)所得烧制原料,采用挤出成型机制成所需形状的试件,再放入70℃的鼓风干燥箱中干燥18h,制得SiC质柴油车颗粒捕集器素胚;
3)烧制
将步骤2)所得素胚放入高温炉中,抽真空或充入惰性气体,首先以8℃/min的速度升温至850℃,保温3h,再以13℃/min的速度升温至2110℃,保温1.5h,完成后随炉冷却至室温,制得SiC质柴油车颗粒捕集器。
经测试,本实施例所得SiC质柴油车颗粒捕集器,过滤器通道壁厚0.22mm,开孔率48%,抗压强度30MPa,热膨胀系数1.7×10-6℃-1。
上述实施例只为说明本发明的技术构思及特点,其目的在于让熟悉此项技术的人士能够了解本发明的内容并据以实施,并不能以此限制本发明的保护范围。凡根据本发明精神实质所作的等效变化或修饰,都应涵盖在本发明的保护范围之内。
Claims (8)
1.一种SiC质柴油车颗粒捕集器,其特征在于,首先将萜烯树脂、松节油、柴油、邻苯二甲酸二乙酯进行剪切处理制备成型剂,然后以SiC粉末、金属硅粉和成型剂为原料进行混料、干燥、挤压成型和烧制而成;
所述萜烯树脂、松节油、柴油、邻苯二甲酸二乙酯的质量比为100:(50~70):(20~40):(2~3);
挤压成型步骤中进行鼓风干燥,鼓风干燥温度为60~80℃,时间为12~24h;
烧制步骤包括:将挤压成型所得素胚在真空或惰性气氛条件下,首先以6~10℃/min的速率升温至800~900℃,保温2~4h,再以10~15℃/min的速率升温至2080~2150℃,保温1~1.5h,随炉冷却至室温,即得所述SiC质柴油车颗粒捕集器。
2.根据权利要求1所述的SiC质柴油车颗粒捕集器,其特征在于,所述SiC粉末、金属硅和成型剂的质量比为100:(5~10):(10~15)。
3.根据权利要求1~2任一项所述SiC质柴油车颗粒捕集器的制备方法,其特征在于,具体包括如下步骤:
1)烧制原料制备
将萜烯树脂、松节油、柴油、邻苯二甲酸二乙酯按比例混合,进行剪切处理,得成型剂;然后将SiC粉末、金属硅粉和成型剂搅拌混合均匀,干燥,得烧制原料;
2)素胚成型
将所得烧制原料进行挤出成型得到所需形状的试件,再进行鼓风干燥,得成型后的素胚;
3)烧制
将所得素胚在真空或惰性气氛条件下,首先以6~10℃/min的速率升温至800~900℃,保温2~4h,再以10~15℃/min的速率升温至2080~2150℃,保温1~1.5h,随炉冷却至室温,即得所述SiC质柴油车颗粒捕集器。
4.根据权利要求3所述的制备方法,其特征在于,所述萜烯树脂、松节油、柴油、邻苯二甲酸二乙酯的质量比为100:(50~70):(20~40):(2~3)。
5.根据权利要求3所述的制备方法,其特征在于,所述剪切处理温度为105~120℃条件下,剪切速率为200~300r/min,时间为20~25min。
6.根据权利要求3所述的制备方法,其特征在于,所述SiC粉末、金属硅和成型剂的质量比100:(5~10):(10~15)。
7.根据权利要求3所述的制备方法,其特征在于,所述柴油为5#、0#或者-10#柴油。
8.根据权利要求3所述的制备方法,其特征在于,所述SiC粉末的平均粒度为5~40μm,纯度大于97%;所述金属硅粉平均粒径<80μm,硅含量>95%。
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