CN113999021B - 一种可控形貌的镁基耐火材料杂质改性方法 - Google Patents

一种可控形貌的镁基耐火材料杂质改性方法 Download PDF

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CN113999021B
CN113999021B CN202111225499.2A CN202111225499A CN113999021B CN 113999021 B CN113999021 B CN 113999021B CN 202111225499 A CN202111225499 A CN 202111225499A CN 113999021 B CN113999021 B CN 113999021B
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崔妍
曲殿利
刘新
郭玉香
李国华
田琳
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University of Science and Technology Liaoning USTL
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Abstract

本发明涉及一种可控形貌的镁基耐火材料杂质改性方法，包括以下步骤：1)制备镁基材耐火材料的低熔点杂质相钙镁橄榄石；2)在步骤1)的钙镁橄榄石粉体中加入改性剂La2O3进行混合，并干燥；3)将混合好的物料放入压片机中压制成型并干燥；4)将干燥后的试样，置入1300℃以上的高温炉中反应烧结。本发明的优点是：工艺流程简单，成本低，形貌可控制，对低品位菱镁矿进行杂质改性处理，提高了其综合利用率，节约能源。

Description

一种可控形貌的镁基耐火材料杂质改性方法
技术领域
本发明属于耐火材料杂质改性过程控制领域，尤其涉及一种可控形貌的镁基耐火材料杂质改性方法。
背景技术
氧化镁(MgO)具有高熔点，抗碱性渣侵蚀能力强等优点，广泛应用于钢铁冶金、有色金属冶炼和水泥等行业。天然菱镁矿是获得氧化镁的重要来源之一。然而，由于菱镁矿资源的粗放经营，导致优质资源相对短缺，而占我国菱镁矿储量1/3的低品位菱镁矿(氧化镁含量35％～42％)资源却被闲置或废弃堆放，造成资源极大浪费，也导致生态破坏和环境污染。因此对低品位菱镁矿开发利用迫在眉睫。
低品位菱镁矿由于硅钙等杂质含量高而难以满足生产耐火材料和高性能镁化工材料的要求，不能直接使用。普通镁质耐火材料中方镁石晶粒间是由低熔点的硅酸盐相组成，且在方镁石晶粒间连续分布。在高温下低熔点的硅酸盐相先行软化或形成液相，显著降低镁质耐火材料的高温使用性能和抗渣侵蚀性能。为此，要从根本上改善镁质耐火材料性能，应对其显微结构进行设计和改进，对镁砂中方镁石晶界相进行改性，即减少或消除低熔点硅酸盐相、改变硅酸盐相在晶粒间的连续分布状态、提高硅酸盐相的耐火度。这不仅可以提高低品位菱镁矿的综合利用率，拓宽镁质材料的应用领域，还可以节约能源，降低污染，保护环境。
发明内容
为克服现有技术的不足，本发明的目的是提供一种可控形貌的镁基耐火材料杂质改性方法，工艺流程简单，形貌可控制，获得改性效果优良、显微组织形貌可控的新型杂质改性方法。
为实现上述目的，本发明通过以下技术方案实现：
一种可控形貌的镁基材耐火材料杂质改性方法，包括以下步骤：
1)制备镁基材耐火材料的低熔点杂质相钙镁橄榄石；
2)在步骤1)的钙镁橄榄石粉体中加入改性剂La2O3进行混合，并干燥；
3)将混合好的物料放入压片机中压制成型并干燥；
4)将干燥后的试样，置入1300℃以上的高温炉中反应烧结。
步骤1)所述的钙镁橄榄石以CaO、SiO2、MgO分析纯试剂为原料，采用高温固相反应法合成，按照生成钙镁橄榄石CaO·MgO·SiO2的反应方程式制备，反应方程式为：
MgO+CaO+SiO2＝CaO·MgO·SiO2。
所述的CaO、SiO2、MgO分析纯试剂按摩尔比n(CaO:SiO2:MgO)＝1:1:1的比例混合，所述的高温固相法的反应温度控制在1400±10℃，并在1400±10℃保温5h以上。
步骤2)所述的改性剂La2O3占钙镁橄榄石粉体与改性剂La2O3的混合物的重量百分比为10wt％～30wt％，以无水乙醇为介质，以300～350r/min的速度球磨混合5h以上。
步骤3)中在压片机中压制成
Figure BDA0003314145280000021
的柱状试样。
步骤4)中干燥后的试样置入高温炉，在空气气氛中1300～1400℃进行反应烧结，烧结时升温速率为3℃～5℃/min，并在1300～1400℃保温5h以上。
步骤4)中反应烧结的反应方程式如下：
3(CaO·MgO·SiO2)+2La2O3＝CaO·3SiO2·2La2O3+3MgO+2CaO。
与现有技术相比，本发明的有益效果是：
本发明方法工艺流程简单，成本低，形貌可控制，对低品位菱镁矿进行杂质改性处理，提高了其综合利用率，节约能源，保护环境，按照反应：
3(CaO·MgO·SiO2)+2La2O3＝CaO·3SiO2·2La2O3+3MgO+2CaO，通过调整改性剂La2O3的加入量，获得改性效果优良、显微组织形貌可控的新型杂质改性方法，易于推广应用。
本发明充分利用低品位菱镁矿中CaO和SiO2主要杂质成分，通过引入改性剂，将材料中的低熔点硅酸盐杂质相改性为高熔点的含稀土硅酸盐相。通过控制材料的显微形貌，使其原位反应生成的CaLa4(SiO4)3O呈棒状晶生长，即CaLa4(SiO4)3O晶粒呈现由空心管状晶向棒状晶的转变，起到原位自增韧作用，提高材料的抗热震性。
附图说明
图1是杂质相改性后原位生成的空心管状CaLa4(SiO4)3O晶粒的显微形貌图一。
图2是杂质相改性后原位生成的空心管状CaLa4(SiO4)3O晶粒的显微形貌图二。
图3是杂质相改性后原位生成的棒状CaLa4(SiO4)3O晶粒的显微形貌图。
图4是图3中A处的EDS图谱。
图5是图3中B处的EDS图谱。
具体实施方式
下面结合说明书附图对本发明进行详细地描述，但是应该指出本发明的实施不限于以下的实施方式。
实施例1
可控形貌的镁基耐火材料杂质改性方法，包括以下步骤：
1)以CaO、SiO2和MgO分析纯试剂为原料，将CaO、SiO2和MgO按摩尔比n(CaO:SiO2:MgO)＝1:1:1配比，采用高温固相反应法制备出镁质材料中普遍存在杂质硅酸盐相的钙镁橄榄石(CaO·MgO·SiO2)。
2)杂质硅酸盐相钙镁橄榄石粉体中加入重量百分含量为10％的改性剂La2O3(钙镁橄榄石粉体占90％，La2O3占10％)，以无水乙醇为介质，以300r/min的速度，球磨机中用氧化锆球行星球磨5h，所得的泥浆过100目筛，然后在干燥箱中以60℃的温度烘干24h后得到混合均匀的粉料。
3)将混合均匀的粉体压制成
Figure BDA0003314145280000031
的柱状试样，将成型后的柱状试样置于110℃环境下干燥6～8小时。
4)试样置于高温炉中烧结，升温速率为5℃/min，升温至1300℃并保温3h。
本实施例获得了杂质相改性后原位生成的空心管状CaLa4(SiO4)3O晶粒。在高温条件下，改性剂La2O3可将杂质硅酸盐相钙镁橄榄石(CaO·MgO·SiO2)转变为高熔点相CaLa4(SiO4)3O，按照反应方程式：
3(CaO·MgO·SiO2)+2La2O3＝CaO·3SiO2·2La2O3+3MgO+2CaO
进行杂质改性的反应烧结，原位生成的CaLa4(SiO4)3O晶粒呈针状结构并伴有空心管状的显微形貌，该针状和空心管状晶将对镁基耐火材料起到一定的增韧作用，提高材料的高温力学性能。针状和空心管状的显微结构见图1。
实施例2
可控形貌的镁基耐火材料杂质改性方法，包括以下步骤：
1)以CaO、SiO2和MgO分析纯试剂为原料，将CaO、SiO2和MgO按摩尔比n(CaO:SiO2:MgO)＝1:1:1配比，采用高温固相反应法制备出镁质材料中普遍存在杂质硅酸盐相的钙镁橄榄石(CaO·MgO·SiO2)。
2)杂质硅酸盐相钙镁橄榄石粉体中加入重量百分含量为10％的改性剂La2O3(钙镁橄榄石粉体占90％，La2O3占10％)，以无水乙醇为介质，以300r/min的速度，球磨机中用氧化锆球行星球磨5h，所得的泥浆过100目筛，然后在干燥箱中以60℃的温度烘干24h后得到混合均匀的粉料。
3)将混合均匀的粉体压制成
Figure BDA0003314145280000041
的柱状试样，将成型后的柱状试样置于110℃环境下干燥6～8小时。
4)试样置于高温炉中烧结，升温速率为5℃/min，升温至1350℃并保温5h。
本实施例获得了杂质相改性后原位生成的空心管状CaLa4(SiO4)3O晶粒。在高温条件下，改性剂La2O3可将杂质硅酸盐相钙镁橄榄石(CaO·MgO·SiO2)转变为高熔点相CaLa4(SiO4)3O，按照反应方程式：
3(CaO·MgO·SiO2)+2La2O3＝CaO·3SiO2·2La2O3+3MgO+2CaO
进行杂质改性的反应烧结，随着温度的升高和保温时间的延长，原位生成的CaLa4(SiO4)3O晶粒由之前的针状生长成为空心管状的显微形貌，该管状晶将对镁基耐火材料起到良好的增韧作用，提高材料的高温力学性能。空心管状晶体的显微结构见图2。
实施例3
可控形貌的镁基耐火材料杂质改性方法，包括以下步骤：
1)以CaO、SiO2和MgO分析纯试剂为原料，将CaO、SiO2和MgO按摩尔比n(CaO:SiO2:MgO)＝1:1:1配比，采用高温固相反应法制备出镁质材料中普遍存在杂质硅酸盐相的钙镁橄榄石(CaO·MgO·SiO2)。
2)引入重量百分含量为20％的改性剂La2O3，以无水乙醇为介质，以300～350r/min的速度，球磨机中用氧化锆球行星球磨5h，所得的泥浆过100目筛，然后在干燥箱中以60℃的温度烘干24h后得到混合均匀的粉料。
3)将混合均匀的粉体压制成
Figure BDA0003314145280000042
的柱状试样，将成型后的柱状试样置于110℃环境下干燥6～8小时。
4)试样置于高温炉中烧结时升温速率为5℃/min，升温至1400℃并保温5h。
本实施例获得杂质相改性后原位生成的棒状CaLa4(SiO4)3O晶粒。在高温条件下，改性剂La2O3可将杂质硅酸盐相钙镁橄榄石(CaO·MgO·SiO2)转变为高熔点相CaLa4(SiO4)3O，按照反应方程式：
3(CaO·MgO·SiO2)+2La2O3＝CaO·3SiO2·2La2O3+3MgO+2CaO
本实施例对镁基耐火材料杂质改性处理后，在高温条件下，杂质低熔点相钙镁橄榄石(CaO·MgO·SiO2)转变为高熔点相CaLa4(SiO4)3O，并且，随着反应温度的升高和改性剂加入量的增加，原位生成的CaLa4(SiO4)3O空心管状晶体继续向管状中心生长形成棒状晶体的显微形貌，并且晶粒逐渐粗大，该棒状晶引起的桥联将对镁基耐火材料起到更显著的增韧作用，提高材料的高温力学性能。棒状晶体的显微结构见图3-图5。
本发明利用低品位菱镁矿中CaO和SiO2主要杂质成分，通过引入改性剂，将材料中的低熔点硅酸盐杂质相改性为高熔点的含稀土硅酸盐相，并且生成的高熔点相把钙镁橄榄石包裹起来，改性有效。

Claims (4)

1.一种可控形貌的镁基材耐火材料杂质改性方法，其特征在于，包括以下步骤：
1）制备镁基材耐火材料的低熔点杂质相钙镁橄榄石；
所述的钙镁橄榄石以CaO、SiO2、MgO分析纯试剂为原料，采用高温固相反应法合成，按照生成钙镁橄榄石CaO·MgO·SiO2的反应方程式制备，反应方程式为：
MgO+CaO+SiO2 =CaO·MgO·SiO2；
2）在步骤1）的钙镁橄榄石粉体中加入改性剂La2O3进行混合，并干燥；
改性剂La2O3占钙镁橄榄石粉体与改性剂La2O3的混合物的重量百分比为10 wt%～30wt%，以无水乙醇为介质，以300~350 r/min的速度球磨混合5h以上；
3）将混合好的物料放入压片机中压制成型并干燥；
4）将干燥后的试样，置入高温炉，在空气气氛中1300~1400℃进行反应烧结，烧结时升温速率为 3℃~5℃/min，并在1300~1400℃保温5h以上；CaLa4(SiO4)3O晶粒呈现由空心管状晶向棒状晶的转变，起到原位自增韧作用，提高材料的抗热震性。
2.根据权利要求1所述的一种可控形貌的镁基材耐火材料杂质改性方法，其特征在于，所述的CaO、SiO2、MgO分析纯试剂按摩尔比n(CaO:SiO2:MgO)=1:1:1的比例混合，所述的高温固相反应法的反应温度控制在1400±10℃，并在1400±10℃保温5小时以上。
3.根据权利要求1所述的一种可控形貌的镁基材耐火材料杂质改性方法，其特征在于，步骤3）中在压片机中压制成ø20mm×10mm的柱状试样。
4.根据权利要求1所述的一种可控形貌的镁基材耐火材料杂质改性方法，其特征在于，步骤4）中反应烧结的反应方程式如下：
3(CaO·MgO·SiO2)+2La2O3 =CaO·3SiO2·2La2O3+3MgO+2CaO。
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