CN105237014B - 一种轻质微闭孔刚玉复相耐火材料及其制备方法 - Google Patents

一种轻质微闭孔刚玉复相耐火材料及其制备方法 Download PDF

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CN105237014B
CN105237014B CN201510751098.9A CN201510751098A CN105237014B CN 105237014 B CN105237014 B CN 105237014B CN 201510751098 A CN201510751098 A CN 201510751098A CN 105237014 B CN105237014 B CN 105237014B
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CN105237014A (zh
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顾华志
黄奥
付绿平
张美杰
李楠
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Wuhan University of Science and Engineering WUSE
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Abstract

一种轻质微闭孔刚玉复相耐火材料及其制备方法，所述耐火材料，是以95～99重量份数的α‑Al2O3微粉，1～5重量份数的白云石熟料为原料，2～15重量份数的纳米氧化铝溶胶，5～15重量份数的糖类聚合物和30～50重量份数的有机醇为外加剂，混合湿磨得到料浆；然后将料浆置于模具中在15～25℃下放置6～12小时，接着置于60～90℃下保温6～12小时脱模；然后将脱模后的坯体在110～200℃条件下干燥24～36小时，在1800～2000℃条件下保温2～5小时制成。本发明还包括轻质微闭孔刚玉复相耐火材料的制备方法。本发明之轻质微闭孔刚玉复相耐火材料具有体积密度小、平均孔径小、闭口气孔率高、热导率低、热震稳定性好、耐冲刷和抗熔渣侵蚀能力强的特点。

Description

一种轻质微闭孔刚玉复相耐火材料及其制备方法
技术领域
本发明涉及一种刚玉质耐火材料及其制备方法，具体涉及一种轻质微闭孔刚玉复相耐火材料及其制备方法。
背景技术
钢铁是国家工业的基础，钢包是储存、运输与精炼钢水的重要设备，几乎所有新钢种的开发都是在钢包中完成二次精炼的。而耐火材料既是炉衬材料，同时也参与冶金过程，是钢中非金属夹杂和有害元素重要来源之一，也是钢铁冶炼过程中能量消耗的主要通道。因此，耐火材料成为现代钢铁冶炼过程中的关键环节。
目前，耐火材料的损毁主要表现为渣蚀破坏，钢包耐火材料的渣蚀损毁与其它耐火材料相比，其影响因素众多。理论上，熔渣与耐火材料接触首先选择耐火材料气孔等处浸入，如比表面积大、气孔孔径小，此区域容易达到过饱和(阈值)而形成新的化合物。当反应形成高熔点化合物较多时，化合物的附着使耐火材料表面粗糙度增大，浸润加强，循环往复，形成的高熔点化合物增多，最终耐火材料与熔渣之间边界层加厚；当反应形成高熔点化合物较少，也即低熔点化合物较多时，表面粗糙度减小，浸润减弱，如果此时熔渣处于流动状态，熔渣总达不到过饱和度。因此，耐火材料会继续向其中溶解，从而导致耐火材料加剧损毁。大量研究表明，铝镁尖晶石材料在服役过程中，尖晶石捕捉渣中FeO、MnO，刚玉吸收渣的CaO在其表面形成六铝酸钙(简写为CA6)致密层，渣因为SiO2含量相对升高粘度增大。因此，耐火材料的抗渣渗透性和侵蚀性得以增强。张殿军等研究了两种不同碱度的精炼渣下刚玉-尖晶石浇注料的侵蚀行为，结果表明：高碱度渣对浇注料的侵蚀轻微，而低碱度渣与浇注料的渗透反应层较厚。说明不同渣系、渣组成、钢种等冶炼条件下内衬材料抗渣性能的差异性较大，特别是轻量化耐火材料由于体积密度较低，气孔较多，熔渣的扩散通道更多，其渣蚀过程更加复杂。这就要求轻量化的耐火材料具有较多的微闭口气孔和能够在较广泛的渣组成条件下形成抗渣防护层的能力，而目前报道的轻量材料还难以达到要求。因此，研发一种具有高抗渣性能的轻量化耐火材料对于减少钢包耐火材料资源消耗，节约能源，提高冶金生产效率和钢材质量，具有重要的实际意义和应用价值。
发明内容
本发明所要解决的技术问题是，提供一种体积密度小、平均孔径小、闭口气孔率高、热导率低、热震稳定性好、耐冲刷，且能够在较广泛的渣组成条件下形成抗渣防护层能力的轻质微闭孔刚玉复相耐火材料及其制备方法。
本发明解决其技术问题采用的技术方案是，一种轻质微闭孔刚玉复相耐火材料，是以95～99重量份数的α-Al2O3微粉，1～5重量份数的白云石熟料为原料，2～15重量份数的纳米氧化铝溶胶，5～15重量份数的糖类聚合物和30～50重量份数的有机醇为外加剂，混合湿磨得到料浆；然后将料浆置于模具中在15～25℃下放置6～12小时，接着置于60～90℃下保温6～12小时脱模；然后将脱模后的坯体在110～200℃条件下干燥24～36小时，在1800～2000℃条件下保温2～5小时制成。
进一步，所述α-Al2O3微粉的Al2O3含量>99.2wt％，粒径D50为0.5～3μm。
进一步，所述白云石熟料的MgO和CaO总含量>99wt％，粒径D50为2～7μm。
进一步，所述纳米氧化铝溶胶的分散质含量>25wt％，平均粒径为20～50nm。
进一步，所述糖类聚合物为糊精、淀粉、甲壳素中的一种或两种以上的混合物。
进一步，所述有机醇为乙醇、聚乙烯醇、叔丁醇中的一种或两种以上的混合物。
本发明进一步解决其技术问题采用的技术方案是，一种轻质微闭孔刚玉复相耐火材料的制备方法，将α-Al2O3微粉和白云石熟料原料，外加纳米氧化铝溶胶、糖类聚合物和有机醇，混合湿磨0.1～1小时，得到料浆；然后将料浆置于模具中在15～25℃下放置6～12小时，接着置于60～90℃下保温6～12小时脱模；然后将脱模后的坯体在110～200℃条件下干燥24～36小时，在1800～2000℃条件下保温2～5小时，即得轻质微闭孔刚玉复相耐火材料。
进一步，采用行星球磨机湿磨(优选行星球磨机的研磨球为刚玉质球)。
本发明利用纳米氧化铝溶胶的高温超塑性，可使引入白云石熟料中的MgO能够在烧结前期与氧化铝原位反应生成镁铝尖晶石，产生原位相应力有效促使纳米氧化铝超塑性的发挥，使得晶界快速移动，在孔洞被排除之前将其封闭，从而形成大量闭口气孔；而且原位生成的细小镁铝尖晶石能够有效固溶渣中的Fe、Mn等组分，增加熔渣粘度，降低Fe的渗透。此外，引入白云石熟料中的CaO能够在烧结中期与氧化铝原位反应生成六铝酸钙，产生原位相应力促使晶界移动。随着晶界的移动，大孔洞被分割为微小气孔；并且原位生成的细小六铝酸钙能够作为晶种，诱导六铝酸钙生成，从而能够在较广泛的渣组成条件下在骨料周围形成致密的高熔点六铝酸钙等防护层，降低Ca的渗透及其它熔渣组分的侵蚀，整体提升骨料抗渣性能。由此，发明之轻质微闭孔刚玉复相耐火材料具有体积密度小、平均孔径小、闭口气孔率高、热导率低、热震稳定性好、耐冲刷和抗熔渣侵蚀能力强的特点。
实验证明，本发明所制备的轻质微闭孔刚玉复相耐火材料体积密度为2.75～3.05g/cm3，闭口气孔率占总气孔率比例>55％，平均孔径为0.1～0.5μm。
具体实施方式
下面结合实施例对本发明进一步加以说明。
1、原料
α-Al2O3微粉的Al2O3含量>99.2wt％，粒径D50为0.5～3μm。
白云石熟料的MgO和CaO总含量>99wt％，粒径D50为2～7μm。
纳米氧化铝溶胶的分散质含量>25wt％，平均粒径为20～50nm。
行星球磨机的研磨球为刚玉质球。
实施例1：轻质微闭孔刚玉复相耐火材料的制备
以95～97重量份数的α-Al2O3微粉和3～5重量份数的白云石熟料为原料，外加12～15重量份数的纳米氧化铝溶胶、10～15重量份数的糊精和30～40重量份数的乙醇，用行星球磨机混合湿磨0.5～1小时，得到料浆；然后将料浆置于模具中，首先在15～25℃室温条件下放置6～12小时，然后置于60～90℃恒温条件下保温6～12小时，脱模；接着将脱模后的坯体在110～160℃条件下干燥24～30小时，在1900～2000℃条件下保温2～4小时，即得轻质微闭孔刚玉复相耐火材料。
本实施例所制备的轻质微闭孔刚玉复相耐火材料经检测：体积密度为2.75～2.85g/cm3；闭口气孔率占总气孔率比例>55％，平均孔径为0.1～0.3μm。
实施例2：轻质微闭孔刚玉复相耐火材料的制备
以95～97重量份数的α-Al2O3微粉和3～5重量份数的白云石熟料为原料，外加12～15重量份数的纳米氧化铝溶胶、5～10重量份数的淀粉和40～50重量份数的聚乙烯醇，用行星球磨机混合湿磨0.1～0.6小时，得到料浆；然后将料浆置于模具中，首先在15～25℃室温条件下放置6～12小时，然后置于60～90℃恒温条件下保温6～12小时，脱模；接着将脱模后的坯体在150～200℃条件下干燥30～36小时，在1800～1900℃条件下保温3～5小时，即得轻质微闭孔刚玉复相耐火材料。
本实施例所制备的轻质微闭孔刚玉复相耐火材料经检测：体积密度为2.80～2.88g/cm3；闭口气孔率占总气孔率比例>57％，平均孔径为0.2～0.35μm。
实施例3：轻质微闭孔刚玉复相耐火材料的制备
以95～97重量份数的α-Al2O3微粉和3～5重量份数的白云石熟料为原料，外加8～12重量份数的纳米氧化铝溶胶、10～15重量份数的甲壳素和30～40重量份数的叔丁醇，用行星球磨机混合湿磨0.5～1小时，得到料浆；然后将料浆置于模具中，首先在15～25℃室温条件下放置6～12小时，然后置于60～90℃恒温条件下保温6～12小时，脱模；接着将脱模后的坯体在110～160℃条件下干燥24～30小时，在1900～2000℃条件下保温2～4小时，即得轻质微闭孔刚玉复相耐火材料。
本实施例所制备的轻质微闭孔刚玉复相耐火材料经检测：体积密度为2.80～2.85g/cm3；闭口气孔率占总气孔率比例>56％，平均孔径为0.2～0.4μm。
实施例4：轻质微闭孔刚玉复相耐火材料的制备
以95～97重量份数的α-Al2O3微粉和3～5重量份数的白云石熟料为原料，外加占8～12重量份数的纳米氧化铝溶胶、5～10重量份数的糊精和淀粉的混合物和40～50重量份数的乙醇和聚乙烯醇的混合物，用行星球磨机混合湿磨0.1～0.6小时，得到料浆；然后将料浆置于模具中，首先在15～25℃室温条件下放置6～12小时，然后置于60～90℃恒温条件下保温6～12小时，脱模；接着将脱模后的坯体在150～200℃条件下干燥30～36小时，在1800～1900℃条件下保温3～5小时，即得轻质微闭孔刚玉复相耐火材料。
本实施例所制备的轻质微闭孔刚玉复相耐火材料经检测：体积密度为2.90～2.95g/cm3；闭口气孔率占总气孔率比例>57％，平均孔径为0.2～0.4μm。
实施例5：轻质微闭孔刚玉复相耐火材料的制备
以97～99重量份数的α-Al2O3微粉和1～3重量份数的白云石熟料为原料，外加5～8重量份数的纳米氧化铝溶胶、10～15重量份数的糊精和甲壳素的混合物和30～40重量份数的乙醇和叔丁醇中的混合物，用行星球磨机混合湿磨0.5～1小时，得到料浆；然后将料浆置于模具中，首先在15～25℃室温条件下放置6～12小时，然后置于60～90℃恒温条件下保温6～12小时，脱模；接着将脱模后的坯体在110～160℃条件下干燥24～30小时，在1900～2000℃条件下保温2～4小时，即得轻质微闭孔刚玉复相耐火材料。
本实施例所制备的轻质微闭孔刚玉复相耐火材料经检测：体积密度为2.85～2.94g/cm3；闭口气孔率占总气孔率比例>55％，平均孔径为0.25～0.45μm。
实施例6：轻质微闭孔刚玉复相耐火材料的制备
以97～99重量份数的α-Al2O3微粉和1～3重量份数的白云石熟料为原料，外加5～8重量份数的纳米氧化铝溶胶、5～10重量份数的淀粉和甲壳素的混合物和40～50重量份数的聚乙烯醇和叔丁醇中的混合物，用行星球磨机混合湿磨0.1～0.6小时，得到料浆；然后将所述料浆置于模具中，首先在15～25℃室温条件下放置6～12小时，然后置于60～90℃恒温条件下保温6～12小时，脱模；接着将脱模后的坯体在150～200℃条件下干燥30～36小时，在1800～1900℃条件下保温3～5小时，即得轻质微闭孔刚玉复相耐火材料。
本实施例所制备的轻质微闭孔刚玉复相耐火材料经检测：体积密度为2.88～3.00g/cm3；闭口气孔率占总气孔率比例>56％，平均孔径为0.25～0.5μm。
实施例7：轻质微闭孔刚玉复相耐火材料的制备
以97～99重量份数的α-Al2O3微粉和1～3重量份数的白云石熟料为原料，外加2～5重量份数的纳米氧化铝溶胶、10～15重量份数的糊精、淀粉和甲壳素的混合物和30～40重量份数的乙醇、聚乙烯醇和叔丁醇的混合物，用行星球磨机混合湿磨0.5～1小时，得到料浆；然后将料浆置于模具中，首先在15～25℃室温条件下放置6～12小时，然后置于60～90℃恒温条件下保温6～12小时，脱模；接着将脱模后的坯体在110～160℃条件下干燥24～30小时，在1900～2000℃条件下保温2～4小时，即得轻质微闭孔刚玉复相耐火材料。
本实施例所制备的轻质微闭孔刚玉复相耐火材料经检测：体积密度为2.90～3.00g/cm3；闭口气孔率占总气孔率比例>55％，平均孔径为0.3～0.45μm。
实施例8：轻质微闭孔刚玉复相耐火材料的制备
以97～99重量份数的α-Al2O3微粉和1～3重量份数的白云石熟料为原料，外加占所述原料2～5重量份数的纳米氧化铝溶胶、5～10重量份数的糊精、淀粉和甲壳素的混合物和40～50重量份数的乙醇、聚乙烯醇和叔丁醇的混合物，用行星球磨机混合湿磨0.1～0.6小时，得到料浆；然后将所述料浆置于模具中，首先在15～25℃室温条件下放置6～12小时，然后置于60～90℃恒温条件下保温6～12小时，脱模；接着将脱模后的坯体在150～200℃条件下干燥30～36小时，在1800～1900℃条件下保温3～5小时，即得轻质微闭孔刚玉复相耐火材料。
本实施例所制备的轻质微闭孔刚玉复相耐火材料经检测：体积密度为2.95～3.05g/cm3；闭口气孔率占总气孔率比例>55％，平均孔径为0.3～0.5μm。

Claims (9)

1.一种轻质微闭孔刚玉复相耐火材料，其特征在于，是以95～99重量份数的α-Al2O3微粉，1～5重量份数的白云石熟料为原料，2～15重量份数的纳米氧化铝溶胶，5～15重量份数的糖类聚合物和30～50重量份数的有机醇为外加剂，混合湿磨得到料浆；然后将料浆置于模具中在15～25℃下放置6～12小时，接着置于60～90℃下保温6～12小时脱模；然后将脱模后的坯体在110～200℃条件下干燥24～36小时，在1800～2000℃条件下保温2～5小时制成。
2.根据权利要求1所述的轻质微闭孔刚玉复相耐火材料，其特征在于，所述α-Al2O3微粉的Al2O3含量>99.2wt％，粒径D50为0.5～3μm。
3.根据权利要求1所述的轻质微闭孔刚玉复相耐火材料，其特征在于，所述白云石熟料的MgO和CaO总含量>99wt％，粒径D50为2～7μm。
4.根据权利要求1所述的轻质微闭孔刚玉复相耐火材料，其特征在于，所述纳米氧化铝溶胶的分散质含量>25wt％，平均粒径为20～50nm。
5.根据权利要求1所述的轻质微闭孔刚玉复相耐火材料，其特征在于，所述糖类聚合物为糊精、淀粉、甲壳素中的一种或两种以上的混合物。
6.根据权利要求1所述的轻质微闭孔刚玉复相耐火材料，其特征在于，所述有机醇为乙醇、聚乙烯醇、叔丁醇中的一种或两种以上的混合物。
7.一种如权利要求1～6之一所述的轻质微闭孔刚玉复相耐火材料的制备方法，其特征在于，将α-Al2O3微粉和白云石熟料原料，外加纳米氧化铝溶胶、糖类聚合物和有机醇，混合湿磨0.1～1小时，得到料浆；然后将料浆置于模具中在15～25℃下放置6～12小时，接着置于60～90℃下保温6～12小时脱模；然后将脱模后的坯体在110～200℃条件下干燥24～36小时，在1800～2000℃条件下保温2～5小时，即得轻质微闭孔刚玉复相耐火材料。
8.根据权利要求7所述的轻质微闭孔刚玉复相耐火材料的制备方法，其特征在于，采用行星球磨机湿磨。
9.根据权利要求8所述的轻质微闭孔刚玉复相耐火材料的制备方法，其特征在于，所述行星球磨机的研磨球为刚玉质球。
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CN104446543B (zh) * 2014-11-26 2016-08-17 武汉科技大学 一种轻质微闭孔含镁刚玉耐火骨料及其制备方法

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