CN110903097B - 一种原位复合相结合镁铝尖晶石-碳化硅耐火材料的制备方法 - Google Patents
一种原位复合相结合镁铝尖晶石-碳化硅耐火材料的制备方法 Download PDFInfo
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Abstract
本发明属于耐火材料技术领域，公开一种原位复合相结合镁铝尖晶石‑碳化硅耐火材料的制备方法。以镁铝尖晶石颗粒和SiC颗粒作为骨料，碳化硅粉、镁铝尖晶石粉、MgO粉、α‑Al2O3粉和单质Si粉作为基质，将基质部分的镁铝尖晶石粉、碳化硅粉、MgO粉、α‑Al2O3粉和Si粉预混30～50min，将镁铝尖晶石颗粒、SiC颗粒和结合剂混碾10～30min，混合均匀的颗粒料与结合剂内加入预混均匀的基质料，再混碾20～30min，混合料困料、压成生坯并干燥，最后在氮气气氛下烧成得到MgAl2O4‑SiC耐火材料。本发明显著提高了MgAl2O4‑SiC耐火材料的力学性能，降低了煤渣的侵蚀速率。
Description
技术领域
本发明属于耐火材料领域，主要涉及一种原位复合相结合镁铝尖晶石-碳化硅耐火材料的制备方法。
背景技术
目前，水煤浆气化炉用内衬材料为抗侵蚀性优异的高铬耐火材料；但是，由于Cr2O3与CaO、Na2O和K2O发生反应会形成易溶于水的Cr6+，高铬耐火材料在使用过程中存在环境污染的可能性；因此，水煤浆气化炉用无铬耐火材料的研究具有重要意义；目前，国内外针对无铬耐火材料的研究较少，多集中在尖晶石基、氧化铝基、氧化镁基和碳化硅基耐火材料，包括Al2O3-CaO、Al2O3-SiC-C、MgO-MA、非氧化物结合SiC等体系，但这些材料在煤气化特殊环境下均没有表现出较好的抗煤渣侵蚀性。
由于尖晶石质耐火材料具有优异的高温强度和高抗侵蚀性，并且该材料已在钢包内衬、水泥窑、玻璃窑炉和黑液气化等领域得到广泛的应用；而碳化硅材料同样具有优异的抗煤渣渗透性，作为水冷壁气化炉内衬材料已得到很好的应用。因此，笔者的前期研究表明，尖晶石-碳化硅耐火材料是一种潜在的无铬材料，但如何将两种材料结合，是制备该复合材料的关键和难点。
发明内容
本发明的主要目的是提出一种原位复合相结合镁铝尖晶石-碳化硅耐火材料的制备方法，采用原位生成的尖晶石和氮化物复合相作为结合相制备MgAl2O4-SiC耐火材料，通过该方法制备的耐火材料具有优异的力学性能，同时与现有高铬材料相比具有优异的抗煤渣侵蚀性。
为实现以上目的，本发明采用的技术方案如下：
一种原位复合相结合镁铝尖晶石-碳化硅耐火材料的制备方法，制备方法以镁铝尖晶石颗粒和SiC颗粒作为骨料，以碳化硅粉、镁铝尖晶石粉、MgO粉、α-Al2O3粉和单质Si粉作为基质，所述骨料和基质的组成和加入量分别为：镁铝尖晶石颗粒和SiC颗粒60%～75%，SiC粉10%～30%，镁铝尖晶石粉0～10%，MgO和α-Al2O3粉0～5%，单质Si粉5～15%；所述基质与骨料的总质量为100%；将基质部分的镁铝尖晶石粉、碳化硅粉、MgO粉、α-Al2O3粉和Si粉预混30～50min，将镁铝尖晶石颗粒、SiC颗粒和结合剂混碾10～30min，混合均匀的颗粒料与结合剂内加入预混均匀的基质料，再混碾20～30min，混合料困料12～24h后，在液压机上经100～150MPa压成生坯；生坯经110oC干燥4～8h，最后在氮气气氛下经1350～1700oC保温5h烧成得到MgAl2O4-SiC耐火材料。
所述骨料中镁铝尖晶石颗粒为35～75%，SiC颗粒为0～25%。
所述基质中MgO和α-Al2O3粉的配比为生成正尖晶石的化学计量比。
所述结合剂为外加水性树脂，加入量为总质量的3～9%。
所述镁铝尖晶石颗粒为富铝尖晶石，粒度为1～3mm，0.5～1mm和0～0.5mm；配比为：4：2：1。
所述SiC颗粒粒度为1～3mm，0.5～1mm和0～0.5mm三种，配比为：5：3：2。
所述基质中SiC粉的粒度为＜90μm，＜45μm，＜5μm三种，配比为：8：4：3。
所述基质中镁铝尖晶石粉为富铝尖晶石，粒度为＜90μm，＜45μm两种，配比为：3：2。
所述基质中MgO和α-Al2O3粉粒度为325目。
所述基质中Si粉粒度为45μm。
本发明提出的一种原位复合相结合镁铝尖晶石-碳化硅耐火材料的制备方法，采用上述技术方案，具有如下有益效果：
1.将合成镁铝尖晶石和碳化硅复合后，可发挥尖晶石和碳化硅两种材料的互补作用，尖晶石吸收煤灰渣中FeOx，减少其对SiC的氧化，SiC与煤灰渣不润湿，抑制渣的渗透。
2.MgO和α-Al2O3在高温下生成原位镁铝尖晶石，一方面原位尖晶石的形成能够促进烧结，在一定程度上起到结合相的作用，提高材料力学性能；另一方面，原位形成的尖晶石相吸收煤灰渣中FeOx的作用较合成尖晶石更加显著。
3.单质Si粉在流动的氮气气氛下经高温生成了Si3N4、Mg-Sialon等氮化物结合相，显著提高了MgAl2O4-SiC耐火材料的力学性能。同时，该结合相的存在也进一步提高了材料的抗煤渣侵蚀性。
具体实施方式
参照以下实施例对本发明作进一步说明，但本发明不局限于下述实施例。
实施例1：以镁铝尖晶石颗粒和SiC颗粒作为骨料，碳化硅粉、镁铝尖晶石粉、MgO粉、α-Al2O3粉和单质Si粉作为基质，所述骨料和基质的组成和加入量分别为：镁铝尖晶石颗粒和SiC颗粒65%，SiC粉20%，镁铝尖晶石粉10%，MgO和α-Al2O3粉0，单质Si粉5%。将基质部分的镁铝尖晶石粉、碳化硅粉、MgO粉、α-Al2O3粉和Si粉预混30min，将镁铝尖晶石颗粒、SiC颗粒和结合剂混碾15min，混合均匀的颗粒料与结合剂内加入预混均匀的基质料，再混碾20min，混合料困料24h后，在液压机上经110MPa压成生坯；生坯经110oC干燥4h，最后在氮气气氛下经1500oC保温5h烧成得到MgAl2O4-SiC耐火材料。产物的气孔率为18.9 %，常温抗折强度为16.7 MPa。
实施例2：以镁铝尖晶石颗粒和SiC颗粒作为骨料，碳化硅粉、镁铝尖晶石粉、MgO粉、α-Al2O3粉和单质Si粉作为基质，所述骨料和基质的组成和加入量分别为：镁铝尖晶石颗粒和SiC颗粒65%，SiC粉20%，镁铝尖晶石粉7%，MgO和α-Al2O3粉2%，单质Si粉6%。将基质部分的镁铝尖晶石粉、碳化硅粉、MgO粉、α-Al2O3粉和Si粉预混40min，将镁铝尖晶石颗粒、SiC颗粒和结合剂混碾20min，混合均匀的颗粒料与结合剂内加入预混均匀的基质料，再混碾20min，混合料困料12h后，在液压机上经120MPa压成生坯；生坯经110oC干燥6h，最后在氮气气氛下经1600oC保温5h烧成得到MgAl2O4-SiC耐火材料。产物的气孔率为 18.3%，常温抗折强度为17.1 MPa。
实施例3：以镁铝尖晶石颗粒和SiC颗粒作为骨料，碳化硅粉、镁铝尖晶石粉、MgO粉、α-Al2O3粉和单质Si粉作为基质，所述骨料和基质的组成和加入量分别为：镁铝尖晶石颗粒和SiC颗粒65%，SiC粉20%，镁铝尖晶石粉3%，MgO和α-Al2O3粉4%，单质Si粉8%。将基质部分的镁铝尖晶石粉、碳化硅粉、MgO粉、α-Al2O3粉和Si粉预混45min，将镁铝尖晶石颗粒、SiC颗粒和结合剂混碾30min，混合均匀的颗粒料与结合剂内加入预混均匀的基质料，再混碾20min，混合料困料24h后，在液压机上经140MPa压成生坯；生坯经110oC干燥6h，最后在氮气气氛下经1650oC保温5h烧成得到MgAl2O4-SiC耐火材料。产物的气孔率为17.9 %，常温抗折强度为17.7 MPa。
实施例4：以镁铝尖晶石颗粒和SiC颗粒作为骨料，碳化硅粉、镁铝尖晶石粉、MgO粉、α-Al2O3粉和单质Si粉作为基质，所述骨料和基质的组成和加入量分别为：镁铝尖晶石颗粒和SiC颗粒65%，SiC粉20%，镁铝尖晶石粉0，MgO和α-Al2O3粉5%，单质Si粉10%。将基质部分的镁铝尖晶石粉、碳化硅粉、MgO粉、α-Al2O3粉和Si粉预混40min，将镁铝尖晶石颗粒、SiC颗粒和结合剂混碾20min，混合均匀的颗粒料与结合剂内加入预混均匀的基质料，再混碾30min，混合料困料24h后，在液压机上经150MPa压成生坯；生坯经110oC干燥6h，最后在氮气气氛下经1700oC保温5h烧成得到MgAl2O4-SiC耐火材料。产物的显气孔率为17.1%，常温抗折强度也有一定程度的提高，达到17.9MPa。
Claims (2)
1.一种原位复合相结合镁铝尖晶石-碳化硅耐火材料的制备方法，其特征在于：以镁铝尖晶石颗粒和SiC颗粒作为骨料，碳化硅粉、镁铝尖晶石粉、MgO粉、α-Al2O3粉和单质Si粉作为基质，所述骨料和基质的组成和加入量分别为：镁铝尖晶石颗粒和SiC颗粒60%～75%，SiC粉10%～30%，镁铝尖晶石粉0～10%，MgO粉和α-Al2O3粉0～5%，单质Si粉5～15%；所述骨料中镁铝尖晶石颗粒为35～75%，SiC颗粒为0～25%；所述基质与骨料的总质量为100%；将基质部分预混后再与颗粒和结合剂混碾，经困料、压制、干燥，最后在氮气气氛下经1500～1700oC烧成得到MgAl2O4-SiC耐火材料。
2.如权利要求1所述的一种原位复合相结合镁铝尖晶石-碳化硅耐火材料的制备方法，其特征在于：所述基质中MgO粉和α-Al2O3粉的配比为生成正尖晶石的化学计量比。
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| CN107140957A (zh) * | 2017-05-03 | 2017-09-08 | 武汉科技大学 | 一种锌挥发窑用铬刚玉‑镁铝尖晶石砖及其制备方法 |
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