CN110590345A - 一种中频炉用修补料及其制备方法 - Google Patents

一种中频炉用修补料及其制备方法 Download PDF

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CN110590345A
CN110590345A CN201910886884.8A CN201910886884A CN110590345A CN 110590345 A CN110590345 A CN 110590345A CN 201910886884 A CN201910886884 A CN 201910886884A CN 110590345 A CN110590345 A CN 110590345A
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intermediate frequency
frequency furnace
fine powder
repair material
alumina
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张志韧
李亚伟
徐义彪
桑绍柏
姜美平
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Hunan Lida High-New Material Co Ltd
Wuhan University of Science and Engineering WUSE
Wuhan University of Science and Technology WHUST
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Hunan Lida High-New Material Co Ltd
Wuhan University of Science and Engineering WUSE
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Abstract

本发明涉及一种中频炉用修补料及其制备方法。其技术方案是：先以45～65wt％的矾土、5～15wt％的锆刚玉、5～15wt％的红柱石细粉、1～3wt％的氮化硅细粉、10～30wt％的氧化铝微粉、0.5～2wt％的膨润土微粉、1～2wt％的氧化钛细粉、0.5～1wt％的氧化锶微粉和1～2wt％的Ti3AlC2细粉为原料，再外加所述原料0.3～1wt％的硼砂细粉、0.5～1wt％的硼化锆细粉、0.05～0.3wt％的缓凝剂、4～10wt％的硅溶胶和4～10wt％的锆溶胶，湿碾15～30分钟，然后经挤泥机挤泥成型，制得中频炉用修补料。本发明制备的中频炉用修补料不含磷元素、环境友好、粘结性能好、存放时间长、强度高、体积稳定性好、使用寿命长、耐冲刷性能优异和抗侵蚀性能优良。

Description

一种中频炉用修补料及其制备方法
技术领域
本发明属于中频炉用耐火材料技术领域。具体涉及一种中频炉用修补料及其制备方法。
背景技术
中频炉由于具有升温速度快、可间歇作业、操作方便、污染小和高效节能等特点，近年来广泛应用于冶金、铸造等行业，并且不断向大功率、快速熔化和大容量方向发展(蒋伟锋等.一种中频炉修补料结合剂的改进及其应用.工业炉,2014,36(1):pp61～63)。中频炉炉衬是中频炉的重要组成部分，但在生产过程中，炉衬会受到熔融金属和熔渣的冲刷及侵蚀，以及温度频繁变化产生的热冲击，造成炉衬局部产生裂纹或剥落。修补料是一种膏状的耐火材料，将其涂覆在炉衬的裂纹或剥落处，修补料可以与炉衬结合在一起成为一个整体，从而延长炉衬的使用寿命。
目前，中频炉炉衬上使用最为广泛的修补料为高铝质修补料，其(凌志达,等.高铝质耐火可塑料的组成与性能关系研究.南京工业大学学报(自然科学版),1989,11(3):pp8～15)主要采用高铝矾土、氧化铝微粉和结合剂等为原料，经过配料、混炼后封装制备。“一种中频炉炉衬修补用可塑料及其制备方法”(CN106278204)专利技术，该技术以氧化铝、蓝晶石、氧化铬和矾土为原料，以磷酸为结合剂，经混碾和挤泥成型制得中频炉修补用可塑料，该技术主要缺点在于所采用的三氧化二铬会对人和动物的健康安全构成较大威胁，磷酸结合剂会增加冶炼金属中磷元素，且磷酸硬化速度快，难以长期保存。“一种中频炉修补料”(CN108863318A)专利技术，该技术以三氧化铝、三氧化二铬、硼砂、钛白粉和硅微粉为原料，通过引入高温结合剂制备了热态修补性能良好的修补料，但材料中亦含有污染环境的三氧化二铬，常温粘结性能差，加入过多的硼砂及硅微粉不仅使材料烧结后体积收缩过大，导致材料高温强度低及抗冲刷性能差，还会显著降低材料的抗侵蚀性能。
发明内容
本发明旨在克服现有技术缺陷，目的在于提供一种不含磷元素、环境友好、粘结性能好、存放时间长、强度高、体积稳定性好、使用寿命长、耐冲刷性能优异和抗侵蚀性能优良的中频炉用修补料及其制备方法。
为实现上述目的，本发明采用的技术方案是：先以45～65wt％的矾土、5～15wt％的锆刚玉、5～15wt％的红柱石细粉、1～3wt％的氮化硅细粉、10～30wt％的氧化铝微粉、0.5～2wt％的膨润土微粉、1～2wt％的氧化钛细粉、0.5～1wt％的氧化锶微粉和1～2wt％的Ti3AlC2细粉为原料，再外加所述原料0.3～1wt％的硼砂细粉、0.5～1wt％的硼化锆细粉、0.05～0.3wt％的缓凝剂、4～10wt％的硅溶胶和4～10wt％的锆溶胶，湿碾15～30分钟，然后经挤泥机挤泥成型，制得中频炉用修补料。
所述矾土的颗粒级配是：粒径为5～3mm占所述矾土15～30wt％，粒径小于3mm且大于等于1mm占所述矾土15～30wt％，粒径小于1mm且大于等于0.1mm占所述矾土50～60wt％；所述矾土的Al2O3含量﹥76wt％。
所述锆刚玉的颗粒级配是：粒径为3～1mm占所述锆刚玉50～60wt％，粒径小于1mm且大于等于0.5mm占所述锆刚玉15～30wt％，粒径小于0.5mm且大于等于0.1mm占所述锆刚玉15～30wt％；所述锆刚玉的ZrO2含量﹥15wt％。
所述红柱石细粉的Al2O3含量﹥54wt％；红柱石细粉的粒径﹤75μm。
所述氮化硅细粉的Si3N4含量﹥96wt％；氮化硅细粉的粒径﹤45μm。
所述氧化锶微粉的SrO含量﹥97wt％；氧化锶微粉的粒径﹤10μm。
所述的缓凝剂为草酸、六偏磷酸钠和柠檬酸中的一种以上。
所述的锆溶胶的ZrO2含量为15～30wt％，锆溶胶的粒径为20～90nm。
由于采用上述技术方案，本发明与现有技术相比具有如下积极效果：
本发明制备的中频炉用修补料为无铬化耐火材料，不污染环境，对人和动物的健康不会造成潜在威胁，环境友好。
本发明在所制备的中频炉用修补料中加入的膨润土为层状结构，在水中可以分散成增稠性及触变性很好的胶体级粘粒，形成凝胶，使中频炉用修补料具备良好的附着粘结性能。并且，中频炉用修补料中加入了粘性较好的硅溶胶和锆溶胶，进一步提高了中频炉用修补料与炉衬之间的粘结结合程度。利用上述物质的结合特性，本发明制备的中频炉用修补料无需再加入含磷结合剂，避免生产过程中磷污染熔融金属，保证冶炼出的金属具备高的品质，存放时间长。
本发明采用的膨润土由于为层状结构及层间活性阳离子存在，使所制制品在存放过程中能吸附空气中的水分，加之硼砂在空气中也易吸水，保证中频炉用修补料具备良好的保湿性能。中频炉用修补料中加入的缓凝剂及膨润土形成的胶粒赋予了材料优良的触变性，使得中频炉用修补料在较长时间存放后依然具备优良的施工性能。
本发明所制制品在使用过程中，由于其中的硼砂会分解为氧化硼，硼化锆也会氧化为氧化硼，促使中频炉用修补料在较低温度下烧结产生高的强度。高温下，氧化钛会固溶到氧化铝中，能有效促进固相反应和烧结过程，使得骨料与基质紧密结合；同时红柱石会分解为莫来石和石英相，形成的石英相会继续与材料中氧化铝反应生成莫来石，使得材料具备高的强度及优异的耐冲刷性能。
本发明所制制品在高温条件下，莫来石的形成可以产生合适的体积膨胀，抵消中频炉用修补料因烧结而产生的收缩。Ti3AlC2的片状结构可以吸收温度波动产生的热应力，加之锆刚玉中氧化锆及锆溶胶分解产生的氧化锆的增韧作用，赋予了中频炉用修补料优良的体积稳定性及抗热震性能。
本发明制备的修补料中还加入了氮化硅细粉和氧化锶微粉，氮化硅与渣及钢液润湿性差，且能与氧化铝微粉反应生成抗侵蚀性能更优异的塞隆相；同时氧化锶微粉可与其他氧化物及渣作用生成粘度较大的物质沉积在材料表面，使材料具备优异的抗侵蚀性能，有效提高了中频炉用修补料的使用寿命。
本发明所制备的中频炉用修补料经检测：200℃×24h体积密度为2.87～2.97g/cm3，1400℃×4h体积密度为2.82～2.92g/cm3；200℃×24h抗折强度为14～20Mpa，1400℃×4h抗折强度为16～22Mpa；室温下存放120～180天，施工性能不下降；能有效抵抗熔融金属及熔渣对修补料的冲刷和侵蚀20～60炉次。
因此，本发明所制备的中频炉用修补料具有不含磷元素、环境友好、粘结性能好、存放时间长、强度高、体积稳定性好、使用寿命长、耐冲刷性能优异和抗侵蚀性能优良的特点。
具体实施方式
下面结合具体实施方式对本发明作进一步的描述，并非对其保护范围的限制：
为避免重复，先将本具体实施方式所涉及的物料统一描述如下，实施例中不再赘述：
所述矾土的颗粒级配是：粒径为5～3mm占所述矾土15～30wt％，粒径小于3mm且大于等于1mm占所述矾土15～30wt％，粒径小于1mm且大于等于0.1mm占所述矾土50～60wt％；所述矾土的Al2O3含量﹥76wt％。
所述锆刚玉的颗粒级配是：粒径为3～1mm占所述锆刚玉50～60wt％，粒径小于1mm且大于等于0.5mm占所述锆刚玉15～30wt％，粒径小于0.5mm且大于等于0.1mm占所述锆刚玉15～30wt％；所述锆刚玉的ZrO2含量﹥15wt％。
所述红柱石细粉的Al2O3含量﹥54wt％；红柱石细粉的粒径﹤75μm。
所述氮化硅细粉的Si3N4含量﹥96wt％；氮化硅细粉的粒径﹤45μm。
所述氧化锶微粉的SrO含量﹥97wt％；氧化锶微粉的粒径﹤10μm。
所述的缓凝剂为草酸、六偏磷酸钠和柠檬酸中的一种以上。
所述的锆溶胶的ZrO2含量为15～30wt％，锆溶胶的粒径为20～90nm。
实施例1
一种中频炉用修补料及其制备方法。本实施例所述制备方法是：
先以45～55wt％的矾土、5～10wt％的锆刚玉、10～15wt％的红柱石细粉、1～3wt％的氮化硅细粉、20～30wt％的氧化铝微粉、0.5～2wt％的膨润土微粉、1～2wt％的氧化钛细粉、0.5～1wt％的氧化锶微粉和1～2wt％的Ti3AlC2细粉为原料，再外加所述原料0.3～1wt％的硼砂细粉、0.5～1wt％的硼化锆细粉、0.05～0.3wt％的缓凝剂、4～7wt％的硅溶胶和7～10wt％的锆溶胶，湿碾15～25分钟，然后经挤泥机挤泥成型，制得中频炉用修补料。
实施例2
一种中频炉用修补料及其制备方法。本实施例所述制备方法是：
先以48～58wt％的矾土、7～12wt％的锆刚玉、8～13wt％的红柱石细粉、1～3wt％的氮化硅细粉、17～27wt％的氧化铝微粉、0.5～2wt％的膨润土微粉、1～2wt％的氧化钛细粉、0.5～1wt％的氧化锶微粉和1～2wt％的Ti3AlC2细粉为原料，再外加所述原料0.3～1wt％的硼砂细粉、0.5～1wt％的硼化锆细粉、0.05～0.3wt％的缓凝剂、6～9wt％的硅溶胶和5～8wt％的锆溶胶，湿碾17～27分钟，然后经挤泥机挤泥成型，制得中频炉用修补料。
实施例3：
一种中频炉用修补料及其制备方法。本实施例所述制备方法是：
先以51～61wt％的矾土、9～14wt％的锆刚玉、6～11wt％的红柱石细粉、1～3wt％的氮化硅细粉、14～24wt％的氧化铝微粉、0.5～2wt％的膨润土微粉、1～2wt％的氧化钛细粉、0.5～1wt％的氧化锶微粉和1～2wt％的Ti3AlC2细粉为原料，再外加所述原料0.3～1wt％的硼砂细粉、0.5～1wt％的硼化锆细粉、0.05～0.3wt％的缓凝剂、5～8wt％的硅溶胶和6～9wt％的锆溶胶，湿碾19～29分钟，然后经挤泥机挤泥成型，制得中频炉用修补料。
实施例4
一种中频炉用修补料及其制备方法。本实施例所述制备方法是：
先以54～64wt％的矾土、10～15wt％的锆刚玉、5～10wt％的红柱石细粉、1～3wt％的氮化硅细粉、11～21wt％的氧化铝微粉、0.5～2wt％的膨润土微粉、1～2wt％的氧化钛细粉、0.5～1wt％的氧化锶微粉和1～2wt％的Ti3AlC2细粉为原料，再外加所述原料0.3～1wt％的硼砂细粉、0.5～1wt％的硼化锆细粉、0.05～0.3wt％的缓凝剂、7～10wt％的硅溶胶和4～7wt％的锆溶胶，湿碾20～30分钟，然后经挤泥机挤泥成型，制得中频炉用修补料。
实施例5
一种中频炉用修补料及其制备方法。本实施例所述制备方法是：
先以55～65wt％的矾土、8～13wt％的锆刚玉、7～9wt％的红柱石细粉、1～3wt％的氮化硅细粉、10～20wt％的氧化铝微粉、0.5～2wt％的膨润土微粉、1～2wt％的氧化钛细粉、0.5～1wt％的氧化锶微粉和1～2wt％的Ti3AlC2细粉为原料，再外加所述原料0.3～1wt％的硼砂细粉、0.5～1wt％的硼化锆细粉、0.05～0.3wt％的缓凝剂、5～8wt％的硅溶胶和6～9wt％的锆溶胶，湿碾18～28分钟，然后经挤泥机挤泥成型，制得中频炉用修补料。
本具体实施方式与现有技术相比具有如下积极效果：
本具体实施方式制备的中频炉用修补料为无铬化耐火材料，不污染环境，对人和动物的健康不会造成潜在威胁，环境友好。
本具体实施方式在所制备的中频炉用修补料中加入的膨润土为层状结构，在水中可以分散成增稠性及触变性很好的胶体级粘粒，形成凝胶，使中频炉用修补料具备良好的附着粘结性能。并且，中频炉用修补料中加入了粘性较好的硅溶胶和锆溶胶，进一步提高了中频炉用修补料与炉衬之间的粘结结合程度。利用上述物质的结合特性，本具体实施方式制备的中频炉用修补料无需再加入含磷结合剂，避免生产过程中磷污染熔融金属，保证冶炼出的金属具备高的品质，存放时间长。
本具体实施方式采用的膨润土由于为层状结构及层间活性阳离子存在，使所制制品在存放过程中能吸附空气中的水分，加之硼砂在空气中也易吸水，保证中频炉用修补料具备良好的保湿性能。中频炉用修补料中加入的缓凝剂及膨润土形成的胶粒赋予了材料优良的触变性，使得中频炉用修补料在较长时间存放后依然具备优良的施工性能。
本具体实施方式所制制品在使用过程中，由于其中的硼砂会分解为氧化硼，硼化锆也会氧化为氧化硼，促使中频炉用修补料在较低温度下烧结产生高的强度。高温下，氧化钛会固溶到氧化铝中，能有效促进固相反应和烧结过程，使得骨料与基质紧密结合；同时红柱石会分解为莫来石和石英相，形成的石英相会继续与材料中氧化铝反应生成莫来石，使得材料具备高的强度及优异的耐冲刷性能。
本具体实施方式所制制品在高温条件下，莫来石的形成可以产生合适的体积膨胀，抵消中频炉用修补料因烧结而产生的收缩。Ti3AlC2的片状结构可以吸收温度波动产生的热应力，加之锆刚玉中氧化锆及锆溶胶分解产生的氧化锆的增韧作用，赋予了中频炉用修补料优良的体积稳定性及抗热震性能。
本具体实施方式制备的修补料中还加入了氮化硅细粉和氧化锶微粉，氮化硅与渣及钢液润湿性差，且能与氧化铝微粉反应生成抗侵蚀性能更优异的塞隆相；同时氧化锶微粉可与其他氧化物及渣作用生成粘度较大的物质沉积在材料表面，使材料具备优异的抗侵蚀性能，有效提高了中频炉用修补料的使用寿命。
本具体实施方式所制备的中频炉用修补料经检测：200℃×24h体积密度为2.87～2.97g/cm3，1400℃×4h体积密度为2.82～2.92g/cm3；200℃×24h抗折强度为14～20Mpa，1400℃×4h抗折强度为16～22Mpa；室温下存放120～180天，施工性能不下降；能有效抵抗熔融金属及熔渣对修补料的冲刷和侵蚀20～60炉次。
因此，本具体实施方式所制备的中频炉用修补料具有不含磷元素、环境友好、粘结性能好、存放时间长、强度高、体积稳定性好、使用寿命长、耐冲刷性能优异和抗侵蚀性能优良的特点。

Claims (9)

1.一种中频炉用修补料的制备方法，其特征在于：先以45～65wt％的矾土、5～15wt％的锆刚玉、5～15wt％的红柱石细粉、1～3wt％的氮化硅细粉、10～30wt％的氧化铝微粉、0.5～2wt％的膨润土微粉、1～2wt％的氧化钛细粉、0.5～1wt％的氧化锶微粉和1～2wt％的Ti3AlC2细粉为原料，再外加所述原料0.3～1wt％的硼砂细粉、0.5～1wt％的硼化锆细粉、0.05～0.3wt％的缓凝剂、4～10wt％的硅溶胶和4～10wt％的锆溶胶，湿碾15～30分钟，然后经挤泥机挤泥成型，制得中频炉用修补料。
2.根据权利要求1所述的中频炉用修补料的制备方法，其特征在于所述矾土的颗粒级配是：粒径为5～3mm占所述矾土15～30wt％，粒径小于3mm且大于等于1mm占所述矾土15～30wt％，粒径小于1mm且大于等于0.1mm占所述矾土50～60wt％；所述矾土的Al2O3含量﹥76wt％。
3.根据权利要求1所述的中频炉用修补料的制备方法，其特征在于所述锆刚玉的颗粒级配是：粒径为3～1mm占所述锆刚玉50～60wt％，粒径小于1mm且大于等于0.5mm占所述锆刚玉15～30wt％，粒径小于0.5mm且大于等于0.1mm占所述锆刚玉15～30wt％；所述锆刚玉的ZrO2含量﹥15wt％。
4.根据权利要求1所述的中频炉用修补料的制备方法，其特征在于所述红柱石细粉的Al2O3含量﹥54wt％；红柱石细粉的粒径﹤75μm。
5.根据权利要求1所述的中频炉用修补料的制备方法，其特征在于所述氮化硅细粉的Si3N4含量﹥96wt％；氮化硅细粉的粒径﹤45μm。
6.根据权利要求1所述的中频炉用修补料的制备方法，其特征在于所述氧化锶微粉的SrO含量﹥97wt％；氧化锶微粉的粒径﹤10μm。
7.根据权利要求1所述的中频炉用修补料的制备方法，其特征在于所述的缓凝剂为草酸、六偏磷酸钠和柠檬酸中的一种以上。
8.根据权利要求1所述的中频炉用修补料的制备方法，其特征在于所述的锆溶胶的ZrO2含量为15～30wt％，锆溶胶的粒径为20～90nm。
9.一种中频炉用修补料，其特征在于所述中频炉用修补料是根据权利要求1～8项中任一项所述中频炉用修补料的制备方法所制备的中频炉用修补料。
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CN111995375A (zh) * 2020-08-07 2020-11-27 湖南鑫玺新材料有限公司 一种矿热炉用镁质环保炮泥及其制备方法
CN113880561A (zh) * 2021-09-10 2022-01-04 山东泰力克新材料科技有限公司 一种中频感应炉炉衬修补用可塑料及其制备方法
CN114014681A (zh) * 2021-12-08 2022-02-08 湖南仁海科技材料发展有限公司 一种修复刚玉-莫来石推板的方法及修复粘结料
CN116179919A (zh) * 2023-03-07 2023-05-30 宋艺楠 一种纳米金属复合陶瓷材料及其制备方法
CN116283249A (zh) * 2022-12-22 2023-06-23 鞍山钢铁冶金炉材科技有限公司 一种钢包水口座砖热态修补料及其制备、使用方法

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CN116283249A (zh) * 2022-12-22 2023-06-23 鞍山钢铁冶金炉材科技有限公司 一种钢包水口座砖热态修补料及其制备、使用方法
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Application publication date: 20191220