CN111517759A - 一种高热震高抗水化MgO-CaO砂制备方法 - Google Patents

一种高热震高抗水化MgO-CaO砂制备方法 Download PDF

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CN111517759A
CN111517759A CN202010364818.7A CN202010364818A CN111517759A CN 111517759 A CN111517759 A CN 111517759A CN 202010364818 A CN202010364818 A CN 202010364818A CN 111517759 A CN111517759 A CN 111517759A
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cao
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罗旭东
杨孟孟
李季佳
赵嘉亮
王宝林
周晓蕾
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University of Science and Technology Liaoning USTL
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Abstract

本发明涉及一种高热震高抗水化MgO‑CaO砂制备方法，以采用多层炉、悬浮窑、反射窑、回转窑或闪速窑其中一种或多种窑炉类型所生产的轻烧氧化镁粉、轻烧白云石粉为原料，Zr(OH)4干凝胶、TiO2为添加剂，经细磨、混合搅拌、压球、干燥、煅烧得到高热震高抗水化MgO‑CaO砂。本发明MgO‑CaO中以轻烧镁砂和轻烧白云石粉为原料，通过细磨后与Zr(OH)4干凝胶和TiO2混合搅拌压球，煅烧后即可直接制得高热震高抗水化MgO‑CaO砂；ZrO2可与CaO反应生成不易水化的CaZrO3，TiO2与CaO反应生成MgTiO4，提高了制品的抗水化性能；ZrO2引入到基体中，提高了制品的抗热震性能。

Description

一种高热震高抗水化MgO-CaO砂制备方法
技术领域
本发明涉及无机化工技术领域，具体涉及一种高热震高抗水化MgO-CaO砂制备方法。
背景技术
MgO-CaO耐材具有良好的高温稳定性能及抗渣性能，特别是其中游离的CaO可以起到净化钢水的作用，因此，MgO-CaO耐材广泛应用在AOD精炼钢包上。但含钙材料容易水化生成Ca(OH)2引起体积膨胀，进而导致材料损毁，这在很大程度上限制了镁钙材料的使用。
为提高含游离MgO-CaO耐火材料的抗水化性能，一般可以通过物理方法对其包装进行改进，以减少材料与水分的接触；也可以采取在表面形成致密保护层的方式，隔绝耐火原料与空气的接触。目前采用添加其它组分，以在材料中形成低熔点相，促进CaO、MgO晶粒的发育和长大的方法也普遍使用。虽然这些技术手段在一定程度上提高了镁钙材料的抗水化性能，但均以降低MgO-CaO耐火材料的高温使用性能为代价。同时MgO-CaO耐火材料的热震稳定性一直是行业内急待解决的关键技术。
发明内容
本发明针对现有的技术不足，提供了一种高热震高抗水化的MgO-CaO砂制备方法，以轻烧氧化镁粉、轻烧白云石粉为原料，Zr(OH)4干凝胶、TiO2为添加剂，经细磨、混合搅拌、压球、干燥、煅烧，得到一种高热震高抗水化MgO-CaO砂。
为实现上述目的，本发明通过以下技术方案实现：
一种高热震高抗水化MgO-CaO砂制备方法，其特征在于，具体操作步骤如下：
步骤一，以重量份计，将40-50份轻烧氧化镁粉、38-45份轻烧白云石粉细磨至200目以下，得物料细粉；
步骤二，将物料细粉置于混合搅拌机中，以重量份计，将8-15份Zr(OH)2干凝胶细粉和2-4份TiO2微粉均分5-8次加入到混合搅拌机中，混合搅拌10-15min，得混合物料；
步骤三，将混合物料放入压球机中压球，压制成直径40-60mm的MgO-CaO砂球；
步骤四，将MgO-CaO砂球置于100-120℃环境中干燥10-15小时得干燥的MgO-CaO砂球；
步骤五，将干燥的MgO-CaO砂球置于1500-1800℃窑炉中煅烧2-6小时，即得高热震高抗水化MgO-CaO砂；
所述步骤一中的轻烧氧化镁粉和轻烧白云石粉MgO含量³95%。
所述步骤二中的Zr(OH)4干凝胶是氧氯化锆和冰醋酸按8：3的质量比在50-60℃、40kHz下超声波共混20-30min后加氨水调节PH=6，再经50-70℃常压干燥15-20小时制备的。
所述氧氯化锆为含量≥99.0的八水氧氯化锆、冰醋酸为含量98%的冰醋酸、氨水为浓度5%的氨水溶液。
所述步骤五中窑炉为竖窑、回转窑、电窑或隧道窑其中之一。
与现有技术相比，本发明的有益效果是：1）以轻烧镁砂和轻烧白云石粉为原料，通过细磨后与Zr(OH)4干凝胶和TiO2混合搅拌压球，煅烧后即可直接制得高热震高抗水化MgO-CaO砂；2）ZrO2可与CaO反应生成不易水化的CaZrO3，TiO2与CaO反应生成MgTiO4，从而提高了制品的抗水化性能；3）ZrO2引入到MgO-CaO耐火材料的基体中，提高了制品的抗热震性能。
具体实施方式
下面结合实施例对本发明的制备方法做进一步说明：
实施例1：
将50kg轻烧氧化镁粉、40kg轻烧白云石粉细磨至200目以下，得物料细粉；将物料细粉置于混合搅拌机中，将8kgZr(OH)2干凝胶细粉和2kgTiO2微粉均分5次加入到混合搅拌机中，混合搅拌10min，得混合物料；将混合物料放入压球机中压球，压制成直径40mm的MgO-CaO砂球；将MgO-CaO砂球置于100℃环境中干燥4小时，至MgO-CaO砂球中水分含量小于1%，得干燥的MgO-CaO砂球；将干燥的MgO-CaO砂球置于1600℃窑炉中煅烧4小时，即得高热震高抗水化MgO-CaO砂。
经检测本实施例制备的高热震高抗水化MgO-CaO砂：ZrO2与CaO反应生成不易水化的CaZrO3，TiO2与CaO反应生成MgTiO4，并且生成的CaZrO3和MgTiO4主要分布在晶界等容易水化的部位，改变了MgO-CaO材料的显微结构，从而提高了制品的抗水化性能。高温煅烧后的MgO-CaO砂体积密度达到3.33g/cm3；氧化锆晶粒分布于方镁石和方钙石之间的晶界处，提升了MgO-CaO砂的抗热震性能，使MgO-CaO制品热震次数达到10次。
实施例2：
将48kg轻烧氧化镁粉、40kg轻烧白云石粉细磨至200目以下，得物料细粉；将物料细粉置于混合搅拌机中，将10kgZr(OH)2干凝胶细粉和2kgTiO2微粉均分5次加入到混合搅拌机中，混合搅拌10min，得混合物料；将混合物料放入压球机中压球，压制成直径40mm的MgO-CaO砂球；将MgO-CaO砂球置于110℃环境中干燥4小时，至MgO-CaO砂球中水分含量小于1%，得干燥的MgO-CaO砂球；将干燥的MgO-CaO砂球置于1650℃窑炉中煅烧4小时，即得高热震高抗水化MgO-CaO砂。
经检测本实施例制备的高热震高抗水化MgO-CaO砂：ZrO2与CaO反应生成不易水化的CaZrO3，TiO2与CaO反应生成MgTiO4，并且生成的CaZrO3和MgTiO4主要分布在晶界等容易水化的部位，改变了MgO-CaO材料的显微结构，从而提高了制品的抗水化性能。高温煅烧后的MgO-CaO砂体积密度达到3.36g/cm3；氧化锆晶粒分布于方镁石和方钙石之间的晶界处，提升了MgO-CaO砂的抗热震性能，使MgO-CaO制品热震次数达到15次。
实施例3：
将44kg轻烧氧化镁粉、42kg轻烧白云石粉细磨至200目以下，得物料细粉；将物料细粉置于混合搅拌机中，将12kgZr(OH)2干凝胶细粉和2kgTiO2微粉均分5次加入到混合搅拌机中，混合搅拌10min，得混合物料；将混合物料放入压球机中压球，压制成直径40mm的MgO-CaO砂球；将MgO-CaO砂球置于100℃环境中干燥4小时，至MgO-CaO砂球中水分含量小于1%，得干燥的MgO-CaO砂球；将干燥的MgO-CaO砂球置于1800℃窑炉中煅烧4小时，即得高热震高抗水化MgO-CaO砂。
经检测本实施例制备的高热震高抗水化MgO-CaO砂：ZrO2与CaO反应生成不易水化的CaZrO3，TiO2与CaO反应生成MgTiO4，并且生成的CaZrO3和MgTiO4主要分布在晶界等容易水化的部位，改变了MgO-CaO材料的显微结构，从而提高了制品的抗水化性能。高温煅烧后的MgO-CaO砂体积密度达到3.42g/cm3；氧化锆晶粒分布于方镁石和方钙石之间的晶界处，提升了MgO-CaO砂的抗热震性能，使MgO-CaO制品热震次数达到17次。

Claims (4)

1.一种高热震高抗水化MgO-CaO砂制备方法，其特征在于，具体操作步骤如下：
步骤一，以重量份计，将40-50份轻烧氧化镁粉和38-45份轻烧白云石粉细磨至200目以下，得物料细粉；
步骤二，将物料细粉置于混合搅拌机中，以重量份计，将8-15份Zr(OH)2干凝胶细粉和2-4份TiO2微粉均分5-8次加入到混合搅拌机中，混合搅拌10-15min，得混合物料；
步骤三，将混合物料放入压球机中压球，以60-80MPa压制成直径为40-60mm的MgO-CaO砂球；
步骤四，将MgO-CaO砂球置于100-120℃环境中干燥10-15小时得干燥的MgO-CaO砂球；
步骤五，将干燥的MgO-CaO砂球置于1500-1800℃窑炉中煅烧2-6小时，即得高热震高抗水化MgO-CaO砂。
2.根据权利要求1所述一种高热震高抗水化MgO-CaO砂制备方法，其特征在于，所述步骤一中的轻烧氧化镁粉和轻烧白云石粉MgO含量³95%。
3.根据权利要求1所述一种高热震高抗水化MgO-CaO砂制备方法，其特征在于，所述步骤二中的Zr(OH)4干凝胶是氧氯化锆和冰醋酸按8:3的质量比在50-60℃、40kHz下超声波共混20-30min后加氨水调节PH=6，再经50-70℃常压干燥15-20小时制备的；
所述氧氯化锆为含量≥99.0的八水氧氯化锆、冰醋酸为含量98%的冰醋酸、氨水为浓度5%的氨水溶液。
4.根据权利要求1所述一种高热震高抗水化MgO-CaO砂制备方法，其特征在于，所述步骤五中窑炉为竖窑、回转窑、电窑或隧道窑中的任一种。
CN202010364818.7A 2020-04-30 2020-04-30 一种高热震高抗水化MgO-CaO砂制备方法 Pending CN111517759A (zh)

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Application publication date: 20200811