CN110467447B - 一种镁橄榄石晶须增强的镁硅质耐火材料 - Google Patents

一种镁橄榄石晶须增强的镁硅质耐火材料 Download PDF

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CN110467447B
CN110467447B CN201910705005.7A CN201910705005A CN110467447B CN 110467447 B CN110467447 B CN 110467447B CN 201910705005 A CN201910705005 A CN 201910705005A CN 110467447 B CN110467447 B CN 110467447B
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罗旭东
陈娜
李季佳
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University of Science and Technology Liaoning USTL
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Abstract

本发明专利涉及一种镁橄榄石晶须增强的镁硅质耐火材料，以烧结镁橄榄石砂为骨料，以烧结镁砂细粉、烧结镁橄榄石细粉、二氧化硅微粉、氧化镁微粉为基质，以氟化镁细粉作为催化剂，通过混炼、成型、干燥和烧结，可以得到具有镁橄榄石晶须增强的镁硅质耐火材料。本发明制备的镁橄榄石晶须增强的镁硅质耐火材料由资源丰富的MgO、SiO2质原料制备，成本低廉；镁橄榄石晶须具有优良的耐高温、耐腐蚀、优越的热震稳定性和力学性能，将其引入耐火材料可提高耐火材料的韧性、增加冲击强度，有利于提高耐火材料的使用寿命。

Description

一种镁橄榄石晶须增强的镁硅质耐火材料
技术领域
本发明涉及无机化工技术领域，具体涉及一种镁橄榄石晶须增强的镁硅质耐火材料。
背景技术
我国镁硅原料资源丰富，价廉物美，用以开发镁橄榄石质合成原料并制备原位生成镁橄榄石晶须增强的镁硅质耐火材料，可满足钢铁冶金、玻璃、陶瓷等高温工业的需要。镁橄榄石（2MgO·SiO2）属于碱性耐火材料，它与大多数碱性耐火材料的相容性较好，熔点高，达到了1890℃，导热率低，不易水化，有较好的化学稳定性和抵抗金属熔体及渣的侵蚀作用，并且镁橄榄石与钢水直接接触时能保持其稳定性。但天然镁橄榄石中氧化铁含量高，特别是我国的镁橄榄石，氧化铁含量约为7-10%，并且一些铁是以游离态的氧化铁存在，对制品的负面影响更大。开发镁橄榄石合成料，可以减少杂质所带来的负面影响。从耐火材料发展所需要的自然资源上来讲，我国的镁质、硅质资源丰富，随着国家资源的日趋紧张，镁硅矿物的开发及其深度应用也应提上日程。镁橄榄石晶须具有优良的耐高温、耐腐蚀、优越的热震稳定性和力学性能，可以用作耐热构件、高温绝热材料。镁橄榄石石晶须的引入可以提高耐火材料的韧性、增加冲击强度，往往为耐热复合材料研发的首选。因此，本发明方法有效利用在镁硅质耐火材料中生成镁橄榄石晶须，从而提高镁硅质耐火材料的高温力学性能和抗热震稳定性。
发明内容
本发明提供了一种镁橄榄石晶须增强的镁硅质耐火材料，以烧结镁橄榄石砂为骨料，以烧结镁砂细粉、烧结镁橄榄石细粉、二氧化硅微粉、氧化镁微粉为基质，以氟化镁细粉作为催化剂，经混炼、成型、干燥、烧成，得到镁橄榄石晶须增强的镁硅质耐火材料。
为实现上述目的，本发明通过以下技术方案实现：
一种镁橄榄石晶须增强的镁硅质耐火材料，其特征在于，以质量百分比计，以物料总质量60-70%粒径为8-0.074mm的烧结镁橄榄石砂为骨料，以物料总质量5-10%粒径小于0.074mm的烧结镁砂细粉、物料总质量5-10%粒径小于0.074mm的烧结镁橄榄石细粉、物料总质量5-10%粒径小于0.045mm的二氧化硅微粉、物料总质量5-10%粒径为0.045mm的氧化镁微粉为基质，以物料总质量1-5%粒径小于0.074mm的氟化镁细粉作为催化剂，经混炼、成型、干燥和烧成，得到镁橄榄石晶须增强的镁硅质耐火材料，其具体操作步骤如下：
步骤一，将上述烧结镁橄榄石砂骨料置于混炼机中，外加以上述物料总质量5-10%的水，以150-200r/min转速混炼10-20分钟；再加入上述烧结镁砂细粉、烧结镁橄榄石细粉、二氧化硅微粉、氧化镁微粉和氟化镁细粉，以150-200r/min转速继续混炼10-20分钟，得到混炼后的浇注料；
步骤二，成型，将混炼后的浇注料放入模具中进行成型浇注，待样品在模具中养护24-48小时后脱模，得到镁硅质耐火材料坯体；
步骤三，干燥，将脱模后的镁硅质耐火材料坯体于100-150℃的条件下干燥24-48小时；
步骤四，烧成，将干燥后的镁硅质耐火材料坯体从室温升温至1300-1550℃的煅烧温度，保温 2-6小时，随炉自然冷却后取出，即得到镁橄榄石晶须增强的镁硅质耐火材料。
所述步骤四中优选的煅烧温度为1350-1500℃，保温时间为3-5小时。
所述步骤四中从室温升温到煅烧温度过程中的升温速率为1-5℃/min。
与现有技术相比，本发明的有益效果是：1）本发明制备的镁橄榄石晶须增强的镁硅质耐火材料由资源丰富的MgO、SiO2质原料制备，成本低廉；2）镁橄榄石晶须具有优良的耐高温、耐腐蚀、优越的热震稳定性和力学性能，将其引入耐火材料可提高耐火材料的韧性、增加冲击强度，有利于提高耐火材料的使用寿命，晶须可以对砖体起到增韧的作用，晶须的长径比过大增韧效果较差，长径比过小则生成物不能成为晶须，称作晶粒，长径比为20~31之间增强效果最好。
附图说明
图1为本发明的工艺流程示意图。
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：
本实施例给出的一种镁橄榄石晶须增强的镁硅质耐火材料，有以下原料组成：粒径为8-0.074mm的烧结镁橄榄石砂骨料65kg、粒径小于0.074mm的烧结镁砂细粉8kg、粒径小于0.074mm的烧结镁橄榄石细粉8kg、粒径小于0.045mm的二氧化硅微粉8kg、粒径小于0.045mm的氧化镁微粉8kg、粒径小于0.074mm的氟化镁细粉 3kg。通过混炼、成型、干燥和烧成，制备镁橄榄石晶须增强的镁硅质耐火材料，具体操作步骤如下：
步骤一，首先将烧结镁橄榄石砂骨料置于混炼机中，外加7kg水，以150r/min转速混炼20分钟；再加入烧结镁砂细粉、烧结镁橄榄石细粉、二氧化硅微粉、氧化镁微粉和氟化镁细粉，以150r/min转速继续混炼20分钟，得到混炼后的浇注料；
步骤二，成型，将混炼后的浇注料放入模具中进行成型浇注，待样品在模具中养护24小时后脱模，得到镁硅质耐火材料坯体；
步骤三，干燥，将脱模后的镁硅质耐火材料坯体于120℃的条件下干燥25小时；
步骤四，烧成，将干燥后的镁硅质耐火材料坯体于1350℃的高温中煅烧5小时，随炉自然冷却后取出，即得到镁橄榄石晶须增强的镁硅质耐火材料。
本实施例制备的镁硅质耐火材料中的镁铝尖晶石晶须的长径比为21.3，高温抗折强度为13.7MPa，抗热震稳定性为9次。
实施例2：
本实施例给出的一种镁橄榄石晶须增强的镁硅质耐火材料，有以下原料组成：粒径为8-0.074mm的烧结镁橄榄石砂骨料62kg、粒径小于0.074mm的烧结镁砂细粉9kg、粒径小于0.074mm的烧结镁橄榄石细粉9kg、粒径小于0.045mm的二氧化硅微粉9kg、粒径小于0.045mm的氧化镁微粉8kg、粒径小于0.074mm的氟化镁细粉 3kg。通过混炼、成型、干燥和烧成，制备镁橄榄石晶须增强的镁硅质耐火材料，具体操作步骤如下：
步骤一，首先将烧结镁橄榄石砂骨料置于混炼机中，外加10kg水，以150r/min转速混炼15分钟；再加入烧结镁砂细粉、烧结镁橄榄石细粉、二氧化硅微粉、氧化镁微粉和氟化镁细粉，以150r/min转速继续混炼15分钟，得到混炼后的浇注料；
步骤二，成型，将混炼后的浇注料放入模具中进行成型浇注，待样品在模具中养护45小时后脱模，得到镁硅质耐火材料坯体；
步骤三，干燥，将脱模后的镁硅质耐火材料坯体于110℃的条件下干燥35小时；
步骤四，烧成，将干燥后的镁硅质耐火材料坯体于1450℃的高温中煅烧4小时，随炉自然冷却后取出，即得到镁橄榄石晶须增强的镁硅质耐火材料。
本实施例制备的镁硅质耐火材料中的镁铝尖晶石晶须的长径比为30.1，高温抗折强度为17.0MPa，抗热震稳定性为11次。
实施例3：
本实施例给出的一种镁橄榄石晶须增强的镁硅质耐火材料，有以下原料组成：粒径为8-0.074mm的烧结镁橄榄石砂骨料67kg、粒径小于0.074mm的烧结镁砂细粉7kg、粒径小于0.074mm的烧结镁橄榄石细粉7kg、粒径小于0.045mm的二氧化硅微粉7kg、粒径小于0.045mm的氧化镁微粉7kg、粒径小于0.074mm的氟化镁细粉5kg。通过混炼、成型、干燥和烧成，制备镁橄榄石晶须增强的镁硅质耐火材料，具体操作步骤如下：
步骤一，首先将烧结镁橄榄石砂骨料置于混炼机中，外加5kg水，以150r/min转速混炼17分钟；再加入烧结镁砂细粉、烧结镁橄榄石细粉、二氧化硅微粉、氧化镁微粉和氟化镁细粉，以150r/min转速继续混炼17分钟，得到混炼后的浇注料；
步骤二，成型，将混炼后的浇注料放入模具中进行成型浇注，待样品在模具中养护45小时后脱模，得到镁硅质耐火材料坯体；
步骤三，干燥，将养护（脱模）后的镁硅质耐火材料坯体于100℃的条件下干燥36小时；
步骤四，烧成，将干燥后的镁硅质耐火材料坯体于1500℃的高温中煅烧3小时，随炉自然冷却后取出，即得到镁橄榄石晶须增强的镁硅质耐火材料。
本实施例制备的镁硅质耐火材料中的镁铝尖晶石晶须的长径比为27.1，高温抗折强度为15.6MPa，抗热震稳定性为13次。

Claims (3)

1.一种镁橄榄石晶须增强的镁硅质耐火材料，其特征在于，以质量百分比计，以物料总质量60-70%粒径为8-0.074mm的烧结镁橄榄石砂为骨料，以物料总质量5-10%粒径小于0.074mm的烧结镁砂细粉、物料总质量5-10%粒径小于0.074mm的烧结镁橄榄石细粉、物料总质量5-10%粒径小于0.045mm的二氧化硅微粉、物料总质量5-10%粒径为0.045mm的氧化镁微粉为基质，以物料总质量1-5%粒径小于0.074mm的氟化镁细粉作为催化剂，经混炼、成型、干燥和烧成，得到镁橄榄石晶须增强的镁硅质耐火材料，其具体操作步骤如下：
步骤一，将上述烧结镁橄榄石砂骨料置于混炼机中，外加以上述物料总质量5-10%的水，以150-200r/min转速混炼10-20分钟；再加入上述烧结镁砂细粉、烧结镁橄榄石细粉、二氧化硅微粉、氧化镁微粉和氟化镁细粉，以150-200r/min转速继续混炼10-20分钟，得到混炼后的浇注料；
步骤二，成型，将混炼后的浇注料放入模具中进行成型浇注，待样品在模具中养护24-48小时后脱模，得到镁硅质耐火材料坯体；
步骤三，干燥，将脱模后的镁硅质耐火材料坯体于100-150℃的条件下干燥24-48小时；
步骤四，烧成，将干燥后的镁硅质耐火材料坯体从室温升温至1300-1550℃的煅烧温度，保温 2-6小时，随炉自然冷却后取出，即得到镁橄榄石晶须增强的镁硅质耐火材料。
2.根据权利要求1所述的一种镁橄榄石晶须增强的镁硅质耐火材料，其特征在于，所述步骤四中煅烧温度为1350-1500℃，保温时间为3-5小时。
3.根据权利要求1所述的一种镁橄榄石晶须增强的镁硅质耐火材料，其特征在于，所述步骤四中从室温升温到煅烧温度过程中的升温速率为1-5℃/min。
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