CN108727019B - 锆英石砖及其制备方法 - Google Patents

锆英石砖及其制备方法 Download PDF

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CN108727019B
CN108727019B CN201811008280.5A CN201811008280A CN108727019B CN 108727019 B CN108727019 B CN 108727019B CN 201811008280 A CN201811008280 A CN 201811008280A CN 108727019 B CN108727019 B CN 108727019B
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萧子良
刘华利
何承龙
何良德
李盛德
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GUANGZHOU SHIJI REFRACTORY MATERIAL FACTORY
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Abstract

本发明涉及一种锆英石砖及其制备方法。所述的锆英石砖的制备原料包括质量百分为40～60％的致密型锆英石熟料和质量百分为40～60％的基质料；所述的致密型锆英石熟料包括如下质量百分比的各原料：锆英砂78～90％，二氧化锆8～20％，钛白粉0.5～2％；所述的基质料包括如下质量百分比的各原料：锆英砂75～88％，二氧化锆10～20％，钛白粉1～3％，稳定剂0.5～2％，结合剂0.1～0.8％。采用该原料配方制备成的锆英石砖产品，在高温、水雾环境下工作时，不易开裂，具有很好的热震性能和抗侵蚀性能，非常适合用于无碱玻璃纤维熔窑的热应力大或玻璃质量要求高的接触玻璃部位。

Description

锆英石砖及其制备方法
技术领域
本发明涉及耐火材料技术领域，特别是涉及锆英石砖及其制备方法。
背景技术
传统的锆英石砖有采用锆英砂生产，以锆英砂磨成的微粉为原料成型，再烧结后加工为成品。也有一些纯度要求较高的锆英石质砖材，也只是采用精选锆英砂，并通过酸洗、煅烧等一些方法除杂后作为原料来生产。还有一些传统的锆英石砖，以石英砂和氧化锆为原料，对二者煅烧、粉碎获得石英泥浆和氧化锆泥浆，再将石英泥浆、氧化锆泥浆烘干、打粉、过筛得到石英微粉和氧化锆微粉，然后将其微粉与有机结合剂和添加剂混磨，所得混磨物再经烘干、打粉、过筛、高温煅烧等制备锆英石砖。
但是，这些传统的锆英石砖不能很好的应用于无碱玻璃纤维熔窑的热应力大或玻璃质量要求高的接触玻璃部位，如熔化池挂钩砖、拉丝砖。因为无碱玻璃纤维熔窑的这些玻璃部位，在高温而有水雾环境下工作，对侵蚀及热震性要求非常高。
因此，急需研发一种在高温、水雾环境下工作时具有很好的热震性能和抗腐蚀性能的锆英石砖。
发明内容
基于此，本发明的主要目的是提供一种锆英石砖。该锆英石砖能够在高温、水雾环境下工作，具有很好的热震性和抗腐蚀性。
本发明的目的是通过以下技术方案实现的：
一种锆英石砖，所述的锆英石砖的制备原料包括质量百分为40～60％的致密型锆英石熟料和质量百分为40～60％的基质料；
所述的致密型锆英石熟料包括如下质量百分比的各原料：
锆英砂 78～90％，
二氧化锆 8～20％，
钛白粉 0.5-2％；
所述的基质料包括如下质量百分比的各原料：
Figure BDA0001784484820000021
在其中一些实施例中，所述的致密型锆英石熟料包括如下质量百分比的各原料：
锆英砂 80～90％，
二氧化锆 8～18％，
钛白粉 0.5～2％；
所述的基质料包括如下质量百分比的各原料：
Figure BDA0001784484820000022
Figure BDA0001784484820000031
在其中一些实施例中，所述的致密型锆英石熟料包括如下质量百分比的各原料：
所述的致密型锆英石熟料包括如下质量百分比的各原料：
锆英砂 78～90％，
二氧化锆 8～20％，
钛白粉 0.5-2％；
所述的基质料包括如下质量百分比的各原料：
Figure BDA0001784484820000032
在其中一些实施例中，所述的致密型锆英石熟料包括如下质量百分比的各原料：
锆英砂 80～90％，
二氧化锆 8～18％，
钛白粉 0.5～2％；
所述的基质料包括如下质量百分比的各原料：
Figure BDA0001784484820000033
Figure BDA0001784484820000041
在其中一些实施例中，所述的致密型锆英石熟料包括60～100目的致密型锆英石熟料与大于100目的致密型锆英石熟料的混合物，且二者的质量比为(10～20)：(20～40)；所述的基质料的粒径小于等于5μm。
在其中一些实施例中，所述的致密型锆英石熟料中，60～100目的致密型锆英石熟料与大于100目的致密型锆英石熟料的质量比为(10～15)：(35～40)；所述的基质料的粒径小于等于5μm。
在其中一些实施例中，所述的稳定剂选自氧化钇、氧化镧、氧化铈、氧化镁中的至少一种；所述的结合剂选自工业糊精、桃胶、淀粉、聚乙烯醇中的至少一种。
本发明的另一目的是提供一种上述的锆英石砖的制备方法，包括如下步骤：
制备致密型锆英石熟料：取锆英砂、二氧化锆、钛白粉，研磨、压制成型、煅烧、粉碎，获得所需的致密型锆英石熟料；
制备基质料：取锆英砂、二氧化锆、钛白粉、稳定剂、结合剂，研磨，获得所需的基质料；
制备成型料：将所述的密型锆英石熟料、基质料混匀，出料除杂，获得成型料；
制备锆英石砖：压制成型、高温烧成，获得锆英石砖。
在其中一些实施例中，所述制备致密型锆英石熟料、制备基质料的步骤中，所述的粉碎是将原料粉碎至平均粒度小于等于8μm，所述的压制成型采用100～150Mpa冷等静压成型；所述的煅烧的温度为1450～1620℃。
在其中一些实施例中，所述制备锆英石砖的步骤中，所述的压制成型采用150～250MPa冷等静压成型；所述的高温烧成条件包括：1500～1630℃、6～20小时。
与现有技术相比，本发明具备如下有益效果：
本发明以锆英砂为主要原料，在二氧化锆、钛白粉共同配合下制备成致密型锆英石熟料，并以锆英砂为主要原料，在二氧化锆、钛白粉共同配合下与稳定剂、结合剂一起制备成基质料，致密型锆英石熟料与基质料混合，形成特定原料配方的锆英石砖。采用该原料配方制备成的锆英石砖产品，在高温、水雾环境下工作时，不易开裂，能够实现热震性能和抗玻璃侵蚀性能的很好兼顾，非常适合用于无碱玻璃纤维熔窑的热应力大或玻璃质量要求高的接触玻璃部位。
具体实施方式
为了便于理解本发明，下面将对本发明进行更全面的描述。但是，本发明可以以许多不同的形式来实现，并不限于本文所描述的实施例。相反地，提供这些实施例的目的是使对本发明的公开内容的理解更加透彻全面。
除非另有定义，本文所使用的所有的技术和科学术语与属于本发明的技术领域的技术人员通常理解的含义相同。本文中在本发明的说明书中所使用的术语只是为了描述具体的实施例的目的，不是旨在于限制本发明。本文所使用的术语“和/或”包括一个或多个相关的所列项目的任意的和所有的组合。
本发明实施例的原料均来源于市购原料。
实施例1～2
实施例1和实施例2均提供一种锆英石砖及其制备方法。
锆英石砖的原料配方参见表1
Figure BDA0001784484820000061
锆英石砖的制备方法，包括如下步骤：
第一步：致密型锆英石熟料
根据表1的原料配方取锆英砂(≤60目)、二氧化锆(粒径2～10μm)、钛白粉(粒径3～8μm)；经球磨或搅拌磨湿法研磨，加水适量，研磨料浆平均粒度要求≤8μm，研磨好的料浆经烘干或喷雾干燥后；用冷等静压100～150Mpa成型；隧道窑1450～1620℃高温煅烧，煅烧后的骨料显气孔率≤15％，密度≥4.15g/cm3，骨料冷却出窑后破碎、制粉成粒径分别为60～100目的细粉料，即为致密型锆英石熟料。
第二步：制备基质料
根据表1取锆英砂球粉(中径20～35μm)、锆英砂微粉(中位径2～10μm)、钛白粉(中位径3～8μm)、稳定剂(氧化钇)、结合剂(桃胶)，经球磨或搅拌磨湿法研磨，加水适量，研磨料浆平均粒度要求≤8μm，研磨好的泥浆经烘干或喷雾干燥，控制烘干料水分≤0.8％，获得基质料。基质料的粒径为10～15μm。
第三步：制备成型料
根据表1，取第一步制备的致密型锆英石熟料和第二步制备的基质料，用球磨机混拌均匀，球料比为2:1，获得成型料；具体是采用干式球磨机，基质料与熟料分三等份错开加入，混拌时间为60～90分钟，出料后除铁待成型；
第四步：压制成型
采用150～250MPa冷等静压成型，根据砖坯尺寸的不同，保压5～30分钟。
第五步：高温烧成
隧道窑或梭式窑烧成，烧成温度控制为1500～1630℃，保温6～20小时。
第六步：性能检测，满足化学成分、物理性能要求。
实施例3～4
实施例3和实施例4是实施例1的变化例，相比较于实施例1，实施例3和实施例4对原料配方进行了优化，制备方法与实施例1相同。
锆英石砖的原料配方参见表2。
Figure BDA0001784484820000071
实施例5～6
实施例5和实施例6是实施例1的变化例，相比较于实施例1，实施例5和实施例6对原料配方进行了优化，制备方法与实施例1相同。
锆英石砖的原料配方参见表3。
Figure BDA0001784484820000081
经检测：(1)以上实施例制备的致密型锆英石熟料，其化学成分满足：Zr2O≥70％，SiO2≤29％，TiO2:≤2％，Al2O3≤0.5％。(2)制备的锆英石砖，其化学成分满足：Zr2O≥69％，SiO2≤29％，TiO2≤2％，Al2O3≤0.5％。(3)制备的锆英石砖，其物理性能满足：显气孔率≤13％，体积密度≥4.15g/cm3，冷压强度≥180MPa。
对比例1～2
对比例1：本对比例是实施例1的对比例，相比于实施例1的差别主要在于原料配方中单加入锆英砂，而不加入二氧化锆和钛白粉相配。具体原料配方参见表4。
Figure BDA0001784484820000082
对比例2：本对比例是实施例1的对比例，相比于实施例1的差别主要在于原料配方中加入锆英砂和二氧化锆，而不加入钛白粉相配。具体原料配方参见表5。
Figure BDA0001784484820000091
对以上各例的抗热震性能和静态下抗玻璃液侵蚀的性能进行检测，其中：
(一)静态下抗玻璃液侵蚀性能测试的执行标准为GB 10204-1988，具体包括：
取以上实施例和对比例所得耐火材料作为样品，试样规格为(10±0.05)mm×(10±0.05)mm×(70±0.5)mm；测试玻璃为E玻璃，测试温度1250℃，保温72h，测量液面线侵蚀量为G，测量液面线下二分之一处侵蚀量为H。
(二)抗热震性能的检测执行标准为公司标准，该公司标准的具体操作包括：
取以上实施例和对比例所得耐火材料作为样品，试样规格为(114±0.5)mm×(40±0.5)mm×(40±0.5)mm，每个样品切两条试样试验；参照如下方法测试抗热震性能：
(1)将电炉升温到1100℃，保温30min；
(2)将试样放入炉膛中，不可叠放，试样间隙不小于10mm，保温30min；
(3)前5次重复以下①②步骤，直至试样断裂：
①将试样取出，放在铁板上自然冷却40min；
②放入电炉1100℃×30min；
如果试样不断裂则按4步骤进行第6次；
(4)第6次开始，重复以下①②步骤，直至试样断裂：
①电炉取出后放入水中冷却5min，再放在铁板上40min；
②放入电炉1100℃×30min；
(5)试样在炉内断裂，则该次数不计；若是取出后试样断裂或者放入水中冷却断裂则以0.5次计算。
Figure BDA0001784484820000101
综合所述，本发明以锆英砂为主要原料，在二氧化锆、钛白粉配合下形成致密型锆英石熟料，并以锆英砂为主要原料，在二氧化锆、钛白粉配合下与稳定剂、结合剂一起形成基质料，致密型锆英石熟料与基质料混合，形成特定原料配方的锆英石砖。采用该原料配方制备成的锆英石砖产品，在高温、水雾环境下工作时，不易开裂，具有很好的热震性能和抗玻璃侵蚀性能，非常适合用于无碱玻璃纤维熔窑的热应力大或玻璃质量要求高的接触玻璃部位。
以上所述实施例的各技术特征可以进行任意的组合，为使描述简洁，未对上述实施例中的各个技术特征所有可能的组合都进行描述，然而，只要这些技术特征的组合不存在矛盾，都应当认为是本说明书记载的范围。
以上所述实施例仅表达了本发明的几种实施方式，其描述较为具体和详细，但并不能因此而理解为对发明专利范围的限制。应当指出的是，对于本领域的普通技术人员来说，在不脱离本发明构思的前提下，还可以做出若干变形和改进，这些都属于本发明的保护范围。因此，本发明专利的保护范围应以所附权利要求为准。

Claims (10)

1.一种锆英石砖，其特征在于，所述的锆英石砖的制备原料包括质量百分为40～60％的致密型锆英石熟料和质量百分为40～60％的基质料；
所述的致密型锆英石熟料包括如下质量百分比的各原料：
锆英砂 78～90％，
二氧化锆 8～20％，
钛白粉 0.5～2％；
所述的基质料包括如下质量百分比的各原料：
Figure FDA0001784484810000011
2.根据权利要求1所述的锆英石砖，其特征在于，所述的致密型锆英石熟料包括如下质量百分比的各原料：
锆英砂 80～90％，
二氧化锆 8～18％，
钛白粉 0.5～2％；
所述的基质料包括如下质量百分比的各原料：
Figure FDA0001784484810000012
3.根据权利要求1所述的锆英石砖，其特征在于，所述的致密型锆英石熟料包括如下质量百分比的各原料：
所述的致密型锆英石熟料包括如下质量百分比的各原料：
锆英砂 78～90％，
二氧化锆 8～20％，
钛白粉 0.5-2％；
所述的基质料包括如下质量百分比的各原料：
Figure FDA0001784484810000021
4.根据权利要求1至3任一项所述的锆英石砖，其特征在于，所述的致密型锆英石熟料包括如下质量百分比的各原料：
锆英砂 80～90％，
二氧化锆 8～18％，
钛白粉 0.5～2％；
所述的基质料包括如下质量百分比的各原料：
Figure FDA0001784484810000022
5.根据权利要求1至3任一项所述的锆英石砖，其特征在于，所述的致密型锆英石熟料包括60～100目的致密型锆英石熟料与大于100目的致密型锆英石熟料的混合物，且二者的质量比为(10～20)：(20～40)；所述的基质料的粒径小于等于5μm。
6.根据权利要求5所述的锆英石砖，其特征在于，所述的致密型锆英石熟料中，60～100目的致密型锆英石熟料与大于100目的致密型锆英石熟料的质量比为(10～15)：(35～40)；所述的基质料的粒径小于等于5μm。
7.根据权利要求1至3任一项所述的锆英石砖，其特征在于，所述的稳定剂选自氧化钇、氧化镧、氧化铈、氧化镁中的至少一种；所述的结合剂选自工业糊精、桃胶、淀粉、聚乙烯醇中的至少一种。
8.权利要求1至7任一项所述的锆英石砖的制备方法，其特征在于，包括如下步骤：
制备致密型锆英石熟料：取锆英砂、二氧化锆、钛白粉，研磨、压制成型、煅烧、粉碎，获得所需的致密型锆英石熟料；
制备基质料：取锆英砂、二氧化锆、钛白粉、稳定剂、结合剂，研磨，获得所需的基质料；
制备成型料：将所述的密型锆英石熟料、基质料混匀，出料除杂，获得成型料；
制备锆英石砖：压制成型、高温烧成，获得锆英石砖。
9.根据权利要求8所述的锆英石砖的制备方法，其特征在于，所述制备致密型锆英石熟料、制备基质料的步骤中，所述的粉碎是将原料粉碎至平均粒度小于等于8μm，所述的压制成型采用100～150Mpa冷等静压成型；所述的煅烧的温度为1450～1620℃。
10.根据权利要求8所述的锆英石砖的制备方法，其特征在于，所述制备锆英石砖的步骤中，所述的压制成型采用150～250MPa冷等静压成型；所述的高温烧成条件包括：1500～1630℃、6～20小时。
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