CN107935608B - 使用致密锆英石骨料制备锆英石砖的方法 - Google Patents

使用致密锆英石骨料制备锆英石砖的方法 Download PDF

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CN107935608B
CN107935608B CN201711146148.6A CN201711146148A CN107935608B CN 107935608 B CN107935608 B CN 107935608B CN 201711146148 A CN201711146148 A CN 201711146148A CN 107935608 B CN107935608 B CN 107935608B
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张晓峰
孙文礼
李玉强
张瑛
李志军
郑飞
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Zibo Gongtao New Materials Group Co ltd
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Abstract

本发明涉及一种使用致密锆英石骨料制备锆英石砖的方法，属于耐火材料技术领域。本发明所述的使用致密锆英石骨料制备锆英石砖的方法，是以致密锆英石骨料、锆英砂、锆英粉和锆英石球磨微粉为原料，外加干粉有机结合剂和液体结合剂，通过混料、成型、干燥和烧结，制得所述的锆英石砖。本发明所述的使用致密锆英石骨料制备锆英石砖的方法，其设计科学合理，简单易行，制备的锆英石砖具有较强的耐玻璃液、耐碱侵蚀性能，抗热震性好。

Description

使用致密锆英石骨料制备锆英石砖的方法
技术领域
本发明涉及一种使用致密锆英石骨料制备锆英石砖的方法，属于耐火材料技术领域。
背景技术
耐火材料是玻璃窑炉的主要构建材料，直接影响玻璃窑炉的寿命和玻璃的质量。随着玻璃窑炉设计寿命的延长，对关键部位耐火材料的要求也越来越高。前期玻璃窑炉设计边碹砖使用与碹顶同材质的硅砖，直接放置在电熔锆刚玉胸墙上，由于硅砖与电熔锆刚玉砖在高温时发生共熔，严重影响玻璃窑炉寿命。
中国专利申请201010530953.0(CN 102030546 A)公开了一种含特殊锆英石颗粒的锆英石制品，采用加工致密锆英石砖成品剩余的边角余料经破碎、酸洗、烘干后筛选出来的颗粒，符合耐火材料制品成型工艺要求的坯料紧密堆积原理，大大减少了成型时的层裂问题，并且可以降低原材料消耗，减少废弃物排放，节约成本。所使用的特殊锆英石颗粒中ZrO2≥65％，显气孔率≤2％，吸水率在2％以下。
这种致密骨料是“采用加工致密锆英石砖成品剩余的边角余料经破碎、酸洗、烘干后筛选出来的颗粒”，只有生产致密锆英石产品的个别厂家可以制造。
中国专利申请201010171532.4(CN 101851107 A)公开了一种低碱、低熔洞率、低应力的致密锆英石砖及其制造方法，使用高纯度的锆英砂细粉或超细微粉制备锆英砂致密熟料，然后利用熟料生产大型致密锆英石砖，适用于液晶玻璃成型模具。其熟料不添加烧结助剂，使用细粉或超细微粉压制后1570-1650℃高温烧成，破碎、酸洗、再球磨至≤200目的粉料。使用上述粉料等静压成型，高温烧结得到致密制品。这是锆英石精细陶瓷部件的制造专利，该专利使用超细粉制备熟料，不添加烧结助剂，致密化的烧成温度较高，易于造成锆英粉分解，影响产品高温稳定性能，同时熟料再球磨至200目，等静压成型，制造成本较高、难度较大。
中国专利申请201511011044.4(CN 105481401 A)公开了一种锆英石耐火砖，使用65 份-70份锆英石细粉、12份-15份铬铁矿粉、20份-25份菱镁矿、12份-15份耐火粘土。所制备的锆英石耐火砖抗酸碱侵蚀性能好，应用于锅炉或加热炉内衬。如果用于高温窑炉，则由于锆英石中引入杂质成分过多，影响高温使用性能。
中国专利申请201410668974.7(CN 105669216 A)公开了一种玻璃池窑用高硅质锆英石耐火砖的生产方法。其特征在于：使用原料及其重量百分比为：锆英石精矿砂12-14％、可塑粘土18-20％、熔融石英粉62％，粘结剂6％。锆英石精矿砂和可塑粘土先混料、压制成坯体，经过570-590℃真空煅烧炉煅烧2.5-3小时后，破碎为0.01-0.03mm颗粒，与其他原料混合、机压成型，1400-1450℃保温22-24小时进行烧成。制备所得的高硅质锆英石耐火砖，引入大量石英和可塑粘土，提高了杂质含量，影响锆英石砖的高温性能和抗碱侵蚀性能。
发明内容
本发明的目的在于提供一种使用致密锆英石骨料制备锆英石砖的方法，其设计科学合理，简单易行，制备的锆英石砖具有较强的耐玻璃液、耐碱侵蚀性能，抗热震性好。
本发明所述的使用致密锆英石骨料制备锆英石砖的方法，是以致密锆英石骨料、锆英砂、锆英粉和锆英石球磨微粉为原料，外加干粉有机结合剂和液体结合剂，通过混料、成型、干燥和烧结，制得所述的锆英石砖；
所述的锆英石球磨微粉和致密锆英石骨料的制备方法如下：
(1)以ZrO2≥65％的锆英砂或锆英粉为基础原料，外加钛白粉或其他烧结助剂，经过湿法研磨和干燥，制得锆英石球磨微粉；
(2)步骤(1)所得的锆英石球磨微粉经成型、烧结，制得体积密度＞4.0g/cm3的致密锆英石骨料。
所述的锆英石砖使用的原料的粒度规格及其重量百分比如下：
Figure BDA0001472518140000021
外加入的干粉有机结合剂占上述原料总重量的0.1-0.3％，液体结合剂占上述原料总重量的3-5％。
所述锆英砂和锆英粉的规格为ZrO2≥65％，优选Al2O3≤0.7％、最大Al2O3≤1.2％。
所述干粉有机结合剂为甲基纤维素(CMC)等；液体结合剂为聚乙烯醇或木素磺酸盐溶液。
上述步骤(1)中，使用氧化锆研磨介质或高耐磨度的氧化铝磨介球，在球磨机或搅拌磨等研磨设备中湿法研磨，做成研磨粒度为D50＝1～6μm的泥浆。经过烘干或喷雾干燥，制得锆英石球磨微粉。烧结助剂的加入质量为基础原料质量的0.6％～1.2％。球磨微粉经过50-200MPa 干法等静压成型做成烧成坯体；或球磨微粉添加3～5％的液体结合剂(木质素磺酸盐溶液或聚乙烯醇溶液等)，混炼均匀做成半干法泥料，液压机或摩擦压力机成型成坯体，经过干燥得到烧成坯体；或使用研磨泥浆注入石膏模具内脱水成型，脱模后坯体经过干燥成烧成坯体。
上述步骤(2)中，烧成坯体使用隧道窑或梭式窑，进行1400-1600℃保温10-100小时的烧成，做成体积密度＞4.0g/cm3的致密骨料坯体。经破碎、筛分、磁选，制得0.1～3mm或0.1～5mm的致密锆英石骨料。烧成温度优选为1510～1540℃。
所述的使用致密锆英石骨料制备锆英石砖的方法，包括以下步骤：
(1)先将致密锆英石骨料和锆英砂投入轮碾式混料机混合，再加入液体结合剂混合，然后将锆英粉、锆英石球磨微粉和干粉有机结合剂加入锥式混料机，混合后放入轮碾式混料机中，混合10-20分钟，做成半干法泥料；
(2)将半干法泥料放入成型料仓中困料4-5小时；
(3)使用摩擦压力机或液压机机压成型，成型所得坯体的密度＞3.70g/cm3；
(4)对坯体烘干，使用远红外烘干箱或其他干燥装备，烘干温度为80-120℃，保温24-48 小时；
(5)使用梭式窑或其他烧成窑炉烧成，烧成温度为1400-1600℃，优选为1510～1540℃，保温12-36小时。
制得的锆英石砖的物理指标如下：气孔率≤20％，体积密度≥3.7g/cm3，常温耐压强度≥90MPa，荷重软化点温度(0.2MPa)T1≥1700℃，ZrO2≥64％。
本发明与现有技术相比，具有以下有益效果：
(1)使用体积密度＞4.0g/cm3的致密锆英石骨料、锆英砂和锆英粉为原料，能够得到高的体积密度；
(2)使用的≤6μm的锆英石球磨微粉，可有效充填空隙，提高制品致密度，提高泥料塑性，与有机结合剂一起提供成型性能，高温下容易形成锆英石固相烧结结合，具有较高的常温和高温强度，以及较高的荷重软化点温度；
(3)制得的锆英石砖的耐火度高，荷重软化温度高，热膨胀系数低，导热率随温度的升高而降低，机械强度高，耐玻璃液、耐碱侵蚀性能优良，抗热震性好，在钠钙玻璃熔窑火焰空间与硅砖和电熔铸锆刚玉材料不反应，可安全使用于钠钙玻璃融窑的硅质大碹与AZS胸墙间隔部位，如边碹砖、测温孔砖、观察孔砖等部位，能够有效提高窑炉稳定性，减少热修，延长窑炉寿命；
(4)制备方法简单易行，节能环保，利于大规模工业化生产。
具体实施方式
下面结合实施例对本发明作进一步的说明，但其并不限制本发明的实施。
实施例
1、制备锆英石球磨微粉和致密锆英石骨料：
按照实施例方案配料，使用ZrO2≥65％的锆英粉，添加0.6-1.2％的钛白粉等烧结助剂，在球磨机或搅拌磨等研磨设备中湿法研磨，研磨至粒度D50＝1-6微米泥浆。泥浆经烘干或喷雾造粒制得到锆英石球磨微粉。
对粉料进行50-200MPa等静压成型、半干法压机成型，或泥浆浇注成型成坯体。坯体干燥后使用梭式窑或其他窑炉进行1400-1600℃保温10-100小时烧成，做成体积密度＞4.0g/cm3的骨料坯体。通过破碎、筛分、磁选，制得≤3mm或≤5mm致密锆英石骨料。
制得的致密锆英石骨料的配料比例及体积密度检测结果见表1。
表1
原料名称 粒度 实施例1 实施例2 实施例3 实施例4 实施例5 实施例6
锆英粉 ≤0.045mm 100 100 100 100 100 100
钛白粉 ≤0.045mm 0.6 0.8 1 1.2 1.2 1.2
研磨粒度 μm 2 2 2 2 1 6
体积密度 g/cm3 4.2 4.23 4.31 4.4 4.35 4.33
2、使用致密锆英石骨料制备锆英石砖：
实施例4获得骨料的体积密度最大，使用实施例4获得的致密锆英石骨料制备锆英石砖，具体实施例如下：
使用轮碾式混料机半干法混料。将0～5mm或0～3mm的致密锆英石骨料，以及≤0.1mm 锆英砂投入轮碾式混料机混合均匀；再加入液体结合剂混合均匀；≤0.044mm锆英粉、≤6μm 锆英石球磨微粉和干粉有机结合剂加入锥式混料机，混合均匀后放入轮碾式混料机中，混合 10-20分钟，做成半干法泥料；放入成型料仓中困料4-5小时。
使用摩擦压力机或液压机机压成型，成型密度＞3.70g/cm3。
坯体烘干，使用远红外烘干箱或其他干燥装备，烘干温度为80-120℃。
使用梭式窑或其他烧成窑炉，烧成温度为1400-1600℃，保温12-36小时。
使用致密锆英石骨料制备锆英石砖的配料比例见表2。
表2
Figure BDA0001472518140000041
Figure BDA0001472518140000051
实施例8-14制品的检测结果及化学成分组成见表3和表4。
表3
Figure BDA0001472518140000052
表4
Figure BDA0001472518140000053
。

Claims (1)

1.一种使用致密锆英石骨料制备锆英石砖的方法，其特征在于：包括以下步骤：
（1）制备锆英石球磨微粉和致密锆英石骨料：
按照方案配料，使用ZrO2≥65%的锆英粉，以锆英粉的用量为100wt%计量，添加1.2wt%的钛白粉烧结助剂，在球磨机中湿法研磨，研磨至粒度D50=2微米泥浆；泥浆经喷雾造粒制得到锆英石球磨微粉；锆英粉的粒度≤0.045mm，钛白粉的粒度≤0.045mm；
对粉料进行200MPa等静压成型成坯体；坯体干燥后使用梭式窑进行1600℃保温10小时烧成，做成体积密度4.4g/cm3的骨料坯体；通过破碎、筛分、磁选，制得≤4.75mm致密锆英石骨料；
（2）使用致密锆英石骨料制备锆英石砖：
使用轮碾式混料机半干法混料；将粒度≤4.75mm的致密锆英石骨料40wt%，以及粒度≤0.1mm锆英砂20wt%投入轮碾式混料机混合均匀；再加入PVA 溶液3wt%混合均匀；粒度≤0.045mm锆英粉20wt%、粒度≤0.0065mm锆英石球磨微粉20wt%和粒度≤0.045mm 的CMC0.1wt%加入锥式混料机，混合均匀后放入所述的轮碾式混料机中，混合20分钟，做成半干法泥料；放入成型料仓中困料5小时；PVA 溶液和CMC均为外加物质；
使用液压机机压成型，成型密度＞3.70g/cm3；
坯体烘干，使用远红外烘干箱，烘干温度为120℃；
使用梭式窑或其他烧成窑炉，烧成温度为1600℃，保温36小时。
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