CN108178655A - 一种添加造孔剂工艺制备碳化硅陶瓷过滤器的方法 - Google Patents

一种添加造孔剂工艺制备碳化硅陶瓷过滤器的方法 Download PDF

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CN108178655A
CN108178655A CN201611119995.9A CN201611119995A CN108178655A CN 108178655 A CN108178655 A CN 108178655A CN 201611119995 A CN201611119995 A CN 201611119995A CN 108178655 A CN108178655 A CN 108178655A
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silicon carbide
pore creating
ceramic filter
creating material
powder
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岳鑫
杨殿来
许壮志
胡金玲
高琳琳
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LIAONING FAKU COUNTY CERAMIC ENGINEERING TECHNOLOGY RESEARCH CENTER
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Abstract

本发明涉及一种添加造孔剂工艺制备碳化硅陶瓷过滤器的方法，包括以下步骤：将木屑、碳粉、纤维等低熔点物质中的一种或几种作为造孔剂，添加到以碳化硅为主要成分的复合陶瓷粉体中；通过模压成型的方法，制备得到陶瓷坯体，坯体进行排烧，除去造孔剂得到多孔坯体。多孔坯体经烧结后得到碳化硅陶瓷过滤器。整个过程无需特殊设备，无任何污染，是一种可以制备定向、高孔隙率和高强度陶瓷过滤器的理想工艺。

Description

一种添加造孔剂工艺制备碳化硅陶瓷过滤器的方法
技术领域
本发明涉及一种添加造孔剂工艺制备碳化硅陶瓷过滤器的方法，属于多孔陶瓷领域。
背景技术
随着铸造、化工、冶金、电力等行业的发展，各种高温的液体和气体需要进行过滤处理，以铸造业的钢水过滤为例，使用过滤后的钢水进行铸造可以大幅度的提高成品率，但是钢水的温度极高，一般为可达到1000-1800℃，普通的过滤器无法满足温度要求。在气体的过滤方面，各种工业炉窑所排放出来的高温含尘气体不仅温度高(500～1200℃)，而且含有大量的粉尘(5～30μm)且很强的腐蚀，是造成环境污染的主要因素之一。现阶段的液体的高温过滤器，多为碳化硅泡沫陶瓷过滤器，存在使用寿命短、孔隙大等缺点。高温气体采用布袋除尘/静电除尘等方法，成本高。所以高温条件下，孔隙径小的、可反复使用的液体或气体陶瓷过滤器的开发与利用具有较好的前景。
随着多孔陶瓷研究工作的不断深入，其制备技术也不断丰富、完善。现阶段碳化硅多孔陶瓷过滤器的制备方法常见的有发泡法、添加造孔剂法、有挤压成型法、泡沫浸渍法等。发泡法添加有机或无机造孔剂，通过物理或化学反应产生挥发性气体而产生泡沫，经干燥和烧结后制成多孔陶瓷，不适于制备具有贯通孔隙结构的制品；传统的添加造孔剂法制备多孔陶瓷，其气孔分布均匀性差，不适合制备高孔隙率的制品；挤压成型法制备的多孔陶瓷，其孔形状、孔隙尺寸分布均匀，但不适于制备孔隙尺寸小于1mm的多孔陶瓷；；有机泡沫浸渍法制备多孔陶瓷，其孔尺寸主要取决于有机泡沫体的孔尺寸，其制品不能实现微小颗粒的过滤；由于上述自身的限制，所获得的孔隙尺寸及孔隙率被局限在一定范围内，难以制备微米级孔隙尺寸、高孔隙率、高强度的多孔陶瓷过滤器。
发明内容
针对上述技术现状，本发明的目的是利用添加造孔剂的工艺制备高孔隙率、孔隙定向排列碳化硅瓷过滤器，以满足高温液体或高温含尘气体所需过滤器对孔隙率、孔隙尺寸及强度的要求。本发明制备碳化硅陶瓷过滤器的方法，包括碳化硅复合粉料的制备、压模成型、排烧及烧结等步骤。具体如下：
(1)高性能碳化硅复合粉料的制备
①根据过滤器孔隙情况和强度的要求，将不同粒度的碳化硅粉体、氧化铝及其他辅料如钙、镁、铁、钾、钠、硅的氧化物进行混合，制备出合适的碳化硅粉料；
②依照实际碳化硅陶瓷过滤器所需孔径的大小和分布，填入一种或多种合适的造孔剂，例如碳粉、木屑、纤维等等，在常温、常压下进行搅拌混合；
③加入粘结剂并进行造粒，得到碳化硅复合造粒粉料，粘结剂为桃胶或阿拉伯树胶等。辅料占碳化硅粉体的比例为1％～10％，造孔剂占碳化硅粉体的比例为5-500％，；搅拌混合后加入粘结剂进行造粒，粘结剂占碳化硅粉体的比例为2-5％；
(2)模压成型
按照过滤器的形状要求制备相应的模具，将碳化硅复合造粒粉料进习模压成型。成型压力5-40MPa，保压时间60-900s。脱模后得到过滤器坯体。
(3)排烧
将脱模后的坯体放置于排烧炉中，加热去除造孔剂，使坯体具备一定的强度，避免在操作过程中开裂。根据不同的造孔剂，温度为400-1000℃室温，时间8-48h。
(4)烧结
将坯体放入高温马弗炉内，以2-10℃/min升温至1350-1600℃保温2-8h，然后随炉冷却，得到碳化硅陶瓷过滤器。
使用本发明提供方法制备的碳化硅陶瓷过滤器，具有较高的孔隙率和定向贯通的孔隙结构，开孔孔隙率40-90％之间，孔隙尺寸1-200微米，孔隙高度定向排列，强度0.5-67.5MPa。
综上所述，本发明具有以下优点：
(1)使用造孔剂法制备高孔隙率、孔隙定向排列的微米级孔隙的多孔陶瓷；
(2)高性能碳化硅复合粉体，可以降低碳化硅的烧结温度；
(3)本发明制备的陶瓷过滤器孔隙率40-90％，孔径尺寸1-200微米，孔径大小及孔隙率易于控制；
(4)本发明制备的陶瓷最高使用温度可达1000度以上；
(5)本发明制备的碳化硅陶瓷过滤器，可清理重复使用。
具体实施方式
下面结合具体实施例，进一步阐述本发明。应理解，这些实施例仅用于说明本发明而不用于限制本发明的范围。
实施例1
(1)高性能碳化硅复合粉料的制备
a、将1000g粒度为20微米的碳化硅粉料，与200g氧化铝及氧化硅、氧化钙、氧化镁各10g的辅料进行喷雾造粒，得到碳化硅混合造粒粉。
b、将600g粒度为10微米的碳粉作为造孔剂加入碳化硅混合造粒粉中，在常温、常压下进行搅拌混合，得到碳化硅复合粉料。
c、搅拌混合后加入粘结剂桃胶进行造粒，桃胶占碳化硅粉体的比例为5％，得到碳化硅复合造粒粉料；
(2)模压成型
将碳化硅复合造粒粉料，倒入圆片状模具中，进行模压成型，成型压力25MPa，保压时间120s，脱模后得到坯体。
(3)排烧
将脱模后的多孔坯体放置于排烧炉中，加热去除造孔剂，温度为500℃室温，时间3h，得到过滤器多孔坯体；
(4)烧结
将坯体放入高温马弗炉内，以5℃/min升温至1500℃保温3h，然后随炉冷却，得到碳化硅陶瓷过滤器。
实施例2
(1)高性能碳化硅复合粉料的制备
a、粒度为5微米和20微米的碳化硅粉料各500g，与500g氧化铝及10g氧化硅、5g氧化钙的辅料进行喷雾造粒，得到碳化硅混合造粒粉。
b、将800g粒度为5微米的碳纤维作为造孔剂加入碳化硅混合造粒粉中，在常温、常压下进行搅拌混合，得到碳化硅复合粉料。
c、搅拌混合后加入粘结剂阿拉伯树胶进行造粒，粘结剂占碳化硅粉体的比例为2％，得到碳化硅复合造粒粉料；
(2)模压成型
将碳化硅复合造粒粉料，导入圆柱状模具中，进行模压成型。成型压力40MPa，保压时间300s，脱模后得到过滤器坯体。
(3)排烧
将脱模后的多孔坯体放置于排烧炉中，加热去除造孔剂，温度为800℃室温，时间5h。
(4)烧结
将坯体放入高温马弗炉内，以3℃/min升温至1400℃保温4h，然后随炉冷却，得到碳化硅陶瓷过滤器；
实施例3
(1)高性能碳化硅复合粉料的制备
a、将1000g粒度为5微米的碳化硅粉料，与200g氧化铝及10g氧化硅、20g氧化钙、10g氧化镁、10g氧化钠、20g氧化铁、10g黏土进行喷雾造粒，得到碳化硅混合造粒粉。
b、将600g粒度为10微米的碳粉作为造孔剂加入碳化硅混合造粒粉中，在常温、常压下进行搅拌混合，得到碳化硅复合粉料。
c、搅拌混合后加入粘结剂桃胶进行造粒，桃胶占碳化硅粉体的比例为3％，得到碳化硅复合造粒粉料；
(2)模压成型
将碳化硅复合造粒粉料，倒入圆片状模具中，进行模压成型。成型压力5MPa，保压时间900s，脱模后得到坯体。
(3)排烧
将脱模后的多孔坯体放置于排烧炉中，加热去除造孔剂，温度为400℃室温，时间48h，得到过滤器多孔坯体；
(4)烧结
将坯体放入高温马弗炉内，以2℃/min升温至1600℃保温8h，然后随炉冷却，得到碳化硅陶瓷过滤器。

Claims (4)

1.一种添加造孔剂工艺制备碳化硅陶瓷过滤器的方法，其特征在于，包括以下步骤：(1)高性能碳化硅复合粉料的制备：首先将选用粒径在0.2-500μm范围内的碳化硅粉体和辅料，辅料包括钙、镁、铁、钾、钠、硅的氧化物以及黏土，将所述碳化硅粉体与至少一种辅料进行混合，辅料占碳化硅粉体的比例为1％～10％，混合后进行喷雾造粒，制备出碳化硅混合造粒粉；依照实际碳化硅陶瓷过滤器所需孔径的大小和分布，再将造孔剂填入到上述碳化硅混合造粒粉中，在常温、常压下进行搅拌混合，造孔剂占碳化硅粉体的比例为5-500％，；搅拌混合后加入粘结剂进行造粒，粘结剂占碳化硅粉体的比例为2-5％，得到碳化硅复合造粒粉料；
(2)模压成型:按照碳化硅陶瓷过滤器的形状要求制备相应的模具，将碳化硅复合造粒粉料进行模压成型，脱模后得到过滤器坯体；
(3)排烧：将脱模后得到过滤器坯体置于排烧炉中，加热去除造孔剂，加热温度为400-1000℃室温，时间为8-48h；
(4)烧结：将过滤器坯体放入高温马弗炉内，以2-10℃/min升温至1350-1600℃，保温2-8h，然后随炉冷却，得到碳化硅陶瓷过滤器。
2.根据权利要求1所述的一种添加造孔剂工艺制备碳化硅陶瓷过滤器的方法，其特征在于，所述步骤(1)中的粘结剂为桃胶或阿拉伯树胶。
3.根据权利要求1所述的一种添加造孔剂工艺制备碳化硅陶瓷过滤器的方法，其特征在于，所述步骤(2)中，模压成型的成型压力为5-40MPa，保压时间60-900s。
4.根据权利要求1所述的一种添加造孔剂工艺制备碳化硅陶瓷过滤器的方法，其特征在于，所述步骤(3)中造孔剂为碳粉、木屑、纤维中的一种或几种。
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