CN112573935B - 一种镁橄榄石-镁铝尖晶石质隔热耐火材料的制备方法 - Google Patents

一种镁橄榄石-镁铝尖晶石质隔热耐火材料的制备方法 Download PDF

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CN112573935B
CN112573935B CN202110022530.6A CN202110022530A CN112573935B CN 112573935 B CN112573935 B CN 112573935B CN 202110022530 A CN202110022530 A CN 202110022530A CN 112573935 B CN112573935 B CN 112573935B
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赵飞
李可可
麦海香
朱先忠
刘新红
徐恩霞
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Abstract

一种镁橄榄石‑镁铝尖晶石质隔热耐火材料的制备方法，其特征在于：所述方法包括以下步骤实现：a、按质量百分比将20~30wt%的碳酸镁质原料、30~45wt%的氢氧化铝和25~50wt%的硅石混合，球磨、喷雾造粒后，在1200~1350℃温度下煅烧1~3个小时，得到含低熔点相的多孔小球；b、将步骤a中制备的含低熔点相的多孔小球以20~50wt%的比例加入到氧化镁质材料中，将原料混合均匀后加入1~5wt%的结合剂，在20~100MPa压力下压制成坯体，干燥后，经1500~1600℃保温2~4小时煅烧，冷却后得到镁橄榄石‑镁铝尖晶石质隔热耐火材料。

Description

一种镁橄榄石-镁铝尖晶石质隔热耐火材料的制备方法
技术领域
本发明属于多孔陶瓷或隔热耐火材料技术领域，具体涉及一种镁橄榄石-镁铝尖晶石质隔热耐火材料的制备方法。
背景技术
按高温窑炉的传热机理分析，热面耐火材料的导热系数越小，其蓄热能力就越强，热损失就越少。因此，开发机械强度高、导热系数低、高温性能优良的隔热耐火材料非常迫切。镁橄榄石材料导热系数低（方镁石的1/4~1/3），即使在高温下也能保持良好的隔热性；镁铝尖晶石材料熔点高（2135℃）、力学性能好。镁铝尖晶石和镁橄榄石质材料物相稳定，与碱性耐火材料相容性好，且二者结合能够起到互补的作用。因此，镁铝尖晶石-镁橄榄石质多孔材料是理想的碱性隔热材料。目前，碱性复相隔热耐火材料的研究较少，如发明专利“多孔方镁石-镁橄榄石-尖晶石复合陶瓷材料及其制备方法”（CN 104086206），该专利以菱镁矿细粉、黏土细分和Al(OH)3粉为主要原料，利用菱镁矿和Al(OH)3原位分解产生气孔，但分解温度不易控制，且形成的气孔多为贯通的开口气孔，会降低材料的力学性能。发明专利“一种镁橄榄石-方镁石-尖晶石复相轻质耐火材料及其制备方法”（CN106946558 A）采用轻质材料玻化微珠、粉煤灰漂珠或闭孔珍珠岩等为成孔剂制备多孔材料，这些成孔剂中的氧化铝含量有限，仅能生成少量尖晶石相，不易调控材料中的物相组分；同时这些成孔剂中含有大量的氧化钠、氧化钾、氧化铁等低熔物，对材料的高温性能不利。
发明内容
本发明的目的正是针对上述现有的技术中所存在的不足之处而提供一种制备镁橄榄石-镁铝尖晶石质隔热耐火材料的方法。该制备方法基于原材料在高温下固、液相之间的扩散反应机制成孔、成孔效率高且无污染。用该方法制备的镁橄榄石-镁铝尖晶石质隔热耐火材料中不会有低熔物杂质的引入，气孔结构呈球形且孤立，孔壁间晶体结合紧密，因此力学性能和高温性能优异。
本发明的目的可通过下述技术步骤来实现：
本发明的镁橄榄石-镁铝尖晶石质隔热耐火材料的制备方法所述方法包括以下步骤实现：
a、按质量百分比将20~30wt%的碳酸镁质原料、30~45wt%的氢氧化铝和25~50wt%的硅石混合，球磨、喷雾造粒后，在1200~1350℃温度下煅烧1~3个小时，得到含低熔点相的多孔小球；
b、将步骤a中制备的含低熔点相的多孔小球以20~50wt%的比例加入到氧化镁质材料中，将原料混合均匀后加入1~5wt%的结合剂，在20~100MPa压力下压制成坯体，干燥后，经1500~1600℃保温2~4小时煅烧，冷却后得到镁橄榄石-镁铝尖晶石质隔热耐火材料。
进一步说，步骤 a中所述的碳酸镁质原料取自天然菱镁石或碱式碳酸镁中的任意一种。
步骤a所制备的多孔小球所含的低熔点相为堇青石、假蓝宝石或顽火辉石中的任意一种或两种，多孔小球粒径分布范围为0.044~0.3mm。
步骤 b中所述的氧化镁质原料取自电熔氧化镁、烧结氧化镁或富镁尖晶石细粉中的任意一种，粒径≤0.088mm。
将步骤 a中所述的含低熔点相多孔小球加入到氧化镁质原料中，高温下低熔点相熔融向周围的氧化镁处扩散留下气孔；低熔点物相被MgO反应消耗生成高熔点的镁橄榄石-镁铝尖晶石质隔热耐火材料。
所制备的镁橄榄石-镁铝尖晶石质隔热耐火材料的气孔结构呈球形，体积密度1.3～1.8g/cm3，耐压强度为20～45MPa，荷重软化温度（T0.5）为1570～1650℃。
本发明中首先以碳酸镁、氢氧化铝和二氧化硅为主要原料配制了含低熔点相的多孔小球；将低熔点的多孔小球加入到氧化镁质材料中，高温下多孔小球逐步熔融，并向周围的MgO扩散形成气孔；扩散反应完成后，低熔物被反应消耗生成高熔点的镁橄榄石-镁铝尖晶石复相材料。
所制备的镁橄榄石-镁铝尖晶石质隔热耐火材料经检测：体积密度1.3～1.8g/cm3，耐压强度为20～45MPa，荷重软化温度（T0.5）为1570～1650℃。
本发明有益效果如下：
本发明基于原材料在高温下固、液相之间的扩散反应机制成孔，具有成孔效率高，环境友好和无低熔物杂质引入的特点；所制备的镁橄榄石-镁铝尖晶石质隔热耐火材料物相组成可调控，孔径大小可控，孔壁周围形成发育良好的尖晶石和橄榄石晶体；所制备的多孔材料具有力学性能好、荷重软化温度高、高温体积稳定性好、使用温度高的特点。
附图说明
图1镁橄榄石（M2S）-镁铝尖晶石（MA）质隔热耐火材料显微结构图。
具体实施方式
本发明以下将结合实施例作进一步的描述。
实施例1
步骤a）按照质量百分比将26wt%的碱式碳酸镁、40wt%的氢氧化铝和34wt%的硅石混合，经行星球磨机球磨6h，喷雾造粒后，在110℃干燥箱烘干，经1300℃煅烧2h，制得含堇青石和假蓝宝石物相的多孔小球;
步骤b）将制备的多孔小球以35wt%的比例加入到烧结镁砂中，再加入原料质量之和3wt%的聚乙烯醇溶液作为结合剂，混合均匀，在60MPa的压力下成型，经1550℃煅烧3h，即得到多孔的镁橄榄石-镁铝尖晶石材料;
本实施例所制备的镁橄榄石-镁铝尖晶石质隔热耐火材料经检测：显气孔率48% ,体积密度为1.70g/cm3，荷重软化温度（T0.5）为1576℃。
实施例2
步骤a）：按照质量百分比将20wt%的菱镁石、30wt%的氢氧化铝和50wt%的硅石混合，经行星球磨机球磨6h，喷雾造粒后在110℃干燥箱烘干，然后经1300℃煅烧2h，制得含有堇青石和顽火辉石相的多孔小球;
步骤b）：将合成的多孔小球以40wt%的比例加入到电熔镁砂细粉中，再加入原料质量之和3wt%的聚乙烯醇溶液作为结合剂，混合均匀，在80MPa的压力下成型，经1580℃煅烧3h即得到多孔的镁橄榄石-镁铝尖晶石材料。
本实施例所制备的镁橄榄石-镁铝尖晶石质隔热耐火材料经检测：显气孔率为53%, 体积密度为1.62g/cm3，荷重软化温度（T0.5）为1603℃。
实施例3
步骤a）：按照质量百分比将28wt%的菱镁石、30wt%的氢氧化铝和42wt%的天然石英混合，经行星球磨机球磨6h，喷雾造粒后在110℃干燥箱烘干，然后经1350℃煅烧2h，制得含堇青石相的多孔小球;
步骤b）：将合成的多孔小球以40wt%的比例加入到富镁尖晶石细粉中，再加入原料质量之和3wt%的聚乙烯醇溶液作为结合剂，混合均匀，在60MPa的压力下成型，经1570℃煅烧3h即得到多孔的镁橄榄石-镁铝尖晶石材料。
本实施例所制备的镁橄榄石-镁铝尖晶石质隔热耐火材料经检测：显气孔率为48%, 体积密度为1.70g/cm3，荷重软化温度（T0.5）为1612℃。

Claims (4)

1.一种镁橄榄石-镁铝尖晶石质隔热耐火材料的制备方法，其特征在于：所述方法包括以下步骤实现：
a、按质量百分比将20~30wt%的碳酸镁质原料、30~45wt%的氢氧化铝和25~50wt%的硅石混合，球磨、喷雾造粒后，在1200~1350℃温度下煅烧1~3个小时，得到含低熔点相的多孔小球；所制备的多孔小球所含的低熔点相为堇青石、假蓝宝石或顽火辉石中的任意一种或两种，多孔小球粒径分布范围为0.044~0.3mm；所述的含低熔点相多孔小球加入到氧化镁质原料中，高温下低熔点相熔融向周围的氧化镁处扩散留下气孔；低熔点物相被MgO反应消耗生成高熔点的镁橄榄石-镁铝尖晶石质隔热耐火材料；
b、将步骤a中制备的含低熔点相的多孔小球以20~50wt%的比例加入到氧化镁质材料中，将原料混合均匀后加入1~5wt%的结合剂，在20~100MPa压力下压制成坯体，干燥后，经1500~1600℃保温2~4小时煅烧，冷却后得到镁橄榄石-镁铝尖晶石质隔热耐火材料。
2.根据权利要求1所述的镁橄榄石-镁铝尖晶石质隔热耐火材料的制备方法，其特征在于：步骤 a中所述的碳酸镁质原料取自天然菱镁石或碱式碳酸镁中的任意一种。
3.根据权利要求1所述的一种镁橄榄石-镁铝尖晶石质隔热耐火材料的制备方法，其特征在于：步骤 b中所述的氧化镁质原料取自电熔氧化镁、烧结氧化镁或富镁尖晶石细粉中的任意一种，粒径≤0.088mm。
4.根据权利要求 1所述的镁橄榄石-镁铝尖晶石质隔热耐火材料的制备方法，其特征在于：所制备的镁橄榄石-镁铝尖晶石质隔热耐火材料的气孔结构呈球形，体积密度1.3～1.8g/cm3，耐压强度为20～45MPa，荷重软化温度T0.5为1570～1650℃。
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