CN115477544B - 一种耐腐蚀耐火材料及其制备方法 - Google Patents

一种耐腐蚀耐火材料及其制备方法 Download PDF

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CN115477544B
CN115477544B CN202211342398.8A CN202211342398A CN115477544B CN 115477544 B CN115477544 B CN 115477544B CN 202211342398 A CN202211342398 A CN 202211342398A CN 115477544 B CN115477544 B CN 115477544B
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张姗
董舜杰
阮和平
蒋杰
万志华
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Abstract

本发明公开了一种耐腐蚀耐火材料,其原料按重量份包括:废电瓷80份、偏高岭石10‑20份、铝灰8‑10份、活性氧化铝8‑10份、粘结剂4‑6份。本发明还公开了上述耐腐蚀耐火材料的制备方法,包括如下步骤:将废电瓷、偏高岭石、铝灰、粘结剂混匀后陈化,压制成型,干燥,然后在空气氛围中一次烧结得到中间品;在中间品表面喷涂活性氧化铝溶液,干燥,然后在氮气氛围中二次烧结得到耐腐蚀耐火材料。本发明具有良好的强度和耐腐蚀性能。

Description

一种耐腐蚀耐火材料及其制备方法
技术领域
本发明涉及耐火砖材料技术领域,尤其涉及一种耐腐蚀耐火材料及其制备方法。
背景技术
电瓷材料在各个行业的应用非常广泛,用后的废弃电瓷堆积成山,对环境造成严重污染。由于电瓷废料中含有大量的氧化铝和二氧化硅,可以用来制备耐火材料,但是采用电瓷废料制备的耐火材料,其强度和耐腐蚀性能并不太高。
发明内容
基于背景技术存在的技术问题,本发明提出了一种耐腐蚀耐火材料及其制备方法,本发明具有良好的强度和耐腐蚀性能。
本发明提出了一种耐腐蚀耐火材料,其原料按重量份包括:废电瓷80份、偏高岭石10-20份、铝灰8-10份、活性氧化铝8-10份、粘结剂4-6份。
上述废电瓷在使用前需经多次超声洗涤、干燥处理,以去除污泥等其他杂质。
优选地,废电瓷的粒径为1-2mm、1-0.05mm、<0.05mm。
优选地,粒径为1-2mm的废电瓷、粒径为1-0.05mm的废电瓷、粒径<0.05mm的废电瓷的重量比为1:0.82-0.84:1。
本发明对废电瓷选择适宜粒径,并调节各粒径的重量比,可以降低耐火材料的气孔率,提高其强度。
优选地,偏高岭石的粒径为1-0.05mm。
选用适量的偏高岭石和铝灰相互配合,可以促进晶须桥联,减小孔隙率,阻碍裂纹的扩展,提高耐火材料的韧性和强度。
优选地,废电瓷中氧化铝和二氧化硅的摩尔比为1.8-2:1。
本发明通过调节废电瓷中氧化铝和二氧化硅的摩尔比,并和适量偏高岭石、铝灰相互配合,在烧结过程中生成莫来石,提高耐火材料的强度。
优选地,粘结剂为质量分数为10-15wt%的硅溶胶。
优选地,活性氧化铝的粒径<0.05mm。
本发明还提出了上述耐腐蚀耐火材料的制备方法,包括如下步骤:将废电瓷、偏高岭石、铝灰、粘结剂混匀后陈化,压制成型,干燥,然后在空气氛围中一次烧结得到中间品;在中间品表面喷涂活性氧化铝溶液,干燥,然后在氮气氛围中二次烧结得到耐腐蚀耐火材料。
优选地,一次烧结的程序为:升温至900-1000℃,保温0.5-1h,然后升温至1250-1350℃,保温3.5-4h。
优选地,一次烧结的程序为:以6-8℃/min的速度升温至900-1000℃,保温0.5-1h,然后以4-5℃/min的速度升温至1250-1350℃,保温3.5-4h。
优选地,二次烧结的程序为:升温至1500-1600℃,保温1-2h。
优选地,二次烧结的程序为:以6-8℃/min的速度升温1250-1350℃,然后以4-5℃/min的速度升温至1500-1600℃,保温1-2h。
优选地,活性氧化铝溶液的溶剂为固含量为5-7wt%的酚醛树脂溶液。
本发明先在空气氛围中,一次烧结获得高强度的中间品;然后在中间品表面喷涂活性氧化铝溶液,干燥,然后在氮气氛围中烧结;酚醛树脂在升温过程中生成高活性残炭,高活性残炭与活性氧化铝紧密粘附在中间品的表面和表面孔隙中,在氮气参与下反应生成AlON层,紧密结合在耐火材料表面,提高耐火材料的强度和耐腐蚀性能,并且AlON层可以封堵耐火材料表面的孔隙,防止对耐火材料内部的侵蚀,进一步提高耐腐蚀性能。
适宜的升温速度可以进一步提高耐火材料的强度。
有益效果:
本发明选用废电瓷、偏高岭石、铝灰、粘结剂以适宜比例相互配合,可以提高耐火材料的强度,使用废电瓷作为原料,降低了环境污染和生产成本;并通过适宜的烧结程序,大幅提高耐火材料的强度和耐腐蚀性能。
具体实施方式
下面,通过具体实施例对本发明的技术方案进行详细说明,但是应该明确提出这些实施例用于举例说明,但是不解释为限制本发明的范围。
实施例1
一种耐腐蚀耐火材料,其原料按重量份包括:废电瓷80g、粒径为1-0.05mm的偏高岭石10g、铝灰8g、粒径<0.05mm的活性氧化铝10g、质量分数为10wt%的硅溶胶6g;
其中,废电瓷的粒径为1-2mm、1-0.05mm、<0.05mm;
粒径为1-2mm的废电瓷、粒径为1-0.05mm的废电瓷、粒径<0.05mm的废电瓷的重量比为1:0.82:1;
废电瓷中氧化铝和二氧化硅的摩尔比为2:1。
上述耐腐蚀耐火材料的制备方法,包括如下步骤:将废电瓷、偏高岭石、铝灰、粘结剂混匀后陈化12h,于20MPa压制成型,室温干燥24h,再于60℃烘干12h,然后在空气氛围中一次烧结,冷却至室温得到中间品;其中,一次烧结的程序为:以6℃/min的速度升温至900℃,保温1h,然后以4℃/min的速度升温至1250℃,保温4h;
将活性氧化铝均匀分散在固含量为5wt%的酚醛树脂溶液中,然后喷涂在在中间品表面,60℃烘干,然后在氮气氛围中二次烧结,并在氮气氛围中冷却至室温得到耐腐蚀耐火材料;其中,二次烧结的程序为:以6℃/min的速度升温1250℃,然后以4℃/min的速度升温至1500℃,保温2h。
实施例2
一种耐腐蚀耐火材料,其原料按重量份包括:废电瓷80g、粒径为1-0.05mm的偏高岭石20g、铝灰10g、粒径<0.05mm的活性氧化铝8g、质量分数为15wt%的硅溶胶4g;
其中,废电瓷的粒径为1-2mm、1-0.05mm、<0.05mm;
粒径为1-2mm的废电瓷、粒径为1-0.05mm的废电瓷、粒径<0.05mm的废电瓷的重量比为1:0.84:1;
废电瓷中氧化铝和二氧化硅的摩尔比为1.8:1。
上述耐腐蚀耐火材料的制备方法,包括如下步骤:将废电瓷、偏高岭石、铝灰、粘结剂混匀后陈化12h,于20MPa压制成型,室温干燥24h,再于60℃烘干12h,然后在空气氛围中一次烧结,冷却至室温得到中间品;其中,一次烧结的程序为:以8℃/min的速度升温至1000℃,保温0.5h,然后以5℃/min的速度升温至1350℃,保温3.5h;
将活性氧化铝均匀分散在固含量为7wt%的酚醛树脂溶液中,然后喷涂在在中间品表面,60℃烘干,然后在氮气氛围中二次烧结,并在氮气氛围中冷却至室温得到耐腐蚀耐火材料;其中,二次烧结的程序为:以8℃/min的速度升温1350℃,然后以5℃/min的速度升温至1600℃,保温1h。
实施例3
一种耐腐蚀耐火材料,其原料按重量份包括:废电瓷80g、粒径为1-0.05mm的偏高岭石11g、铝灰9g、粒径<0.05mm的活性氧化铝9g、质量分数为12wt%的硅溶胶5g;
其中,废电瓷的粒径为1-2mm、1-0.05mm、<0.05mm;
粒径为1-2mm的废电瓷、粒径为1-0.05mm的废电瓷、粒径<0.05mm的废电瓷的重量比为1:0.83:1;
废电瓷中氧化铝和二氧化硅的摩尔比为1.9:1。
上述耐腐蚀耐火材料的制备方法,包括如下步骤:将废电瓷、偏高岭石、铝灰、粘结剂混匀后陈化12h,于20MPa压制成型,室温干燥24h,再于60℃烘干12h,然后在空气氛围中一次烧结,冷却至室温得到中间品;其中,一次烧结的程序为:以7℃/min的速度升温至950℃,保温0.8h,然后以4℃/min的速度升温至1300℃,保温4h;
将活性氧化铝均匀分散在固含量为6wt%的酚醛树脂溶液中,然后喷涂在在中间品表面,60℃烘干,然后在氮气氛围中二次烧结,并在氮气氛围中冷却至室温得到耐腐蚀耐火材料;其中,二次烧结的程序为:以7℃/min的速度升温1300℃,然后以4℃/min的速度升温至1600℃,保温1.5h。
对比例1
不进行二次烧结,其他同实施例3。
对比例2
不加偏高岭石和铝灰,将“废电瓷80g”替换成“废电瓷100g”,其他同实施例3。
对实施例1-3和对比例1-2制得耐火材料进行性能检测,结果如表1所示。
表1检测结果
备注:静态坩埚法抗渣实验的具体步骤:将耐火材料压制成坩埚状,在每个坩埚中放入50g渣(渣的化学组成(w)为:Fe2O325.03%、Al2O36.63%、CaO16.13%、SiO29.47%、TiO21.1%、MnO20.2%),放入1500℃电炉内烧结并保温3h,自然冷却后沿坩埚截面切开,测量渣蚀面积,计算渣蚀指数(渣蚀面积/原凹槽轴截面积×100%)。
由表1的结果可以看出,本发明具有良好的强度和耐腐蚀性能。
以上所述,仅为本发明较佳的具体实施方式,但本发明的保护范围并不局限于此,任何熟悉本技术领域的技术人员在本发明揭露的技术范围内,根据本发明的技术方案及其发明构思加以等同替换或改变,都应涵盖在本发明的保护范围之内。

Claims (8)

1.一种耐腐蚀耐火材料,其特征在于,其原料按重量份由:废电瓷80份、偏高岭石10-20份、铝灰8-10份、活性氧化铝8-10份、粘结剂4-6份组成;
废电瓷中氧化铝和二氧化硅的摩尔比为1.8-2:1;
所述耐腐蚀耐火材料的制备方法,包括如下步骤:将废电瓷、偏高岭石、铝灰、粘结剂混匀后陈化,压制成型,干燥,然后在空气氛围中一次烧结得到中间品;在中间品表面喷涂活性氧化铝溶液,干燥,然后在氮气氛围中二次烧结得到耐腐蚀耐火材料;
一次烧结的程序为:升温至900-1000℃,保温0.5-1h,然后升温至1250-1350℃,保温3.5-4h;
二次烧结的程序为:升温至1500-1600℃,保温1-2h;
活性氧化铝溶液的溶剂为固含量为5-7wt%的酚醛树脂溶液;
粘结剂为质量分数为10-15wt%的硅溶胶。
2.根据权利要求1所述耐腐蚀耐火材料,其特征在于,废电瓷的粒径为大于1mm且小于等于2mm、小于等于1mm且大于等于0.05mm、<0.05mm。
3.根据权利要求2所述耐腐蚀耐火材料,其特征在于,粒径为大于1mm且小于等于2mm的废电瓷、粒径为小于等于1mm且大于等于0.05mm的废电瓷、粒径<0.05mm的废电瓷的重量比为1:0.82-0.84:1。
4.根据权利要求1所述耐腐蚀耐火材料,其特征在于,偏高岭石的粒径为1-0.05mm。
5.根据权利要求1所述耐腐蚀耐火材料,其特征在于,活性氧化铝的粒径<0.05mm。
6.一种如权利要求1-5任一项所述耐腐蚀耐火材料的制备方法,其特征在于,包括如下步骤:将废电瓷、偏高岭石、铝灰、粘结剂混匀后陈化,压制成型,干燥,然后在空气氛围中一次烧结得到中间品;在中间品表面喷涂活性氧化铝溶液,干燥,然后在氮气氛围中二次烧结得到耐腐蚀耐火材料。
7.根据权利要求6所述耐腐蚀耐火材料的制备方法,其特征在于,一次烧结的程序为:以6-8℃/min的速度升温至900-1000℃,保温0.5-1h,然后以4-5℃/min的速度升温至1250-1350℃,保温3.5-4h。
8.根据权利要求6所述耐腐蚀耐火材料的制备方法,其特征在于,二次烧结的程序为:以6-8℃/min的速度升温1250-1350℃,然后以4-5℃/min的速度升温至1500-1600℃,保温1-2h。
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