CN108892520A - 一种硅质耐火材料的制备方法 - Google Patents
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Abstract
本发明涉及一种硅质耐火材料的制备方法,属于耐火材料技术领域。本发明以氮化硅铁块体作为耐火骨料,制备了硅质耐火材料,本发明采用无水乙醇和造纸污泥,结合超声波分散以及球磨的方式将纳米二氧化硅粉加入材料中,纳米粉分散于骨料与基质间,促进烧结,填充气孔,提高了材料的常温强度及致密性,造纸污泥中含有纤维,能显著提高材料的抗热震性;本发明中高能球磨主要是使粉末的活性增加,有利于通过机械力诱发离子固态扩散和低温出现液相,促进后期的相转变过程,通过球磨作用,使反应物的比表面积增大,使固‑固反应更容易进行;结合剂选用去离子水,轻烧镁粉遇水水化,生成氢氧化镁,起到粘结作用,且廉价而不带进任何杂质。
Description
技术领域
本发明涉及一种硅质耐火材料的制备方法,属于耐火材料技术领域。
背景技术
硅质耐火材料是指SiO2含量在93%以上、耐火度不低于1500℃的无机非金属材料。主要有硅质不定型耐火材料、熔融石英制品、硅砖等,有良好的高温抗酸渣性。其中,硅质不定形耐火材料是一种不定形状、不经烧成直接可以使用的新型耐火材料,它具有工艺简单、使用方便等优点,近年来在窑炉行业上得到广泛使用。熔融石英耐火制品因其耐火度高、热稳定性好、耐钢水冲刷、使用寿命长等优点,被广泛的应用在钢厂中。根据硅砖用途的不同可分为焦炉用硅砖、热风炉用硅砖、玻璃窑用硅砖等。
在我国硅石资源丰富,常采用纯度较高的硅石作为制备硅质耐火材料的主要原料。硅质制品由于原料不纯往往会引入杂质,某些杂质的存在,不会使制品出现大量液相。但是,当杂质Al2O3含量一旦超过1%,硅质耐火材料内部液相就会急剧增加,各方面性能明显下降。因此,含Al2O3较多的工业废弃物不能用来制备硅质耐火材料。
伴随太阳能产业的发展,对晶体硅片的需求日渐俱增,其切割过程中产生的固体废料也越来越多。这些SiC-Si废料如不进行处理,大量的堆积不仅占用土地,浪费资源,还会造成环境污染,给企业、社会带来巨大压力。但国内外尚未出现利用SiC-Si废料制备硅质、多孔及莫来石质耐火材料的报道。从组成上看,利用SiC-Si废料为主要原料制备硅质、多孔及莫来石质耐火材料是可能的,这为SiC-Si废料的利用提供新的途径。
发明内容
本发明所要解决的技术问题:针对现有硅质耐火材料气密性较差、导热性能及抗热震性能也较低的问题,提供了一种硅质耐火材料的制备方法。
为解决上述技术问题,本发明采用的技术方案是:
按重量份数计,分别称取10~20份轻烧镁粉、30~50份氮化硅铁颗粒、7~12份氮化硅铁粉、5~9份碳化硅粉、1~8份纳米二氧化硅粉、20~30份去离子水、8~16份造纸污泥、10~16份无水乙醇,将纳米二氧化硅粉溶于无水乙醇中,球磨超声波分散后,在温度为60~80℃的烘箱中干燥至恒重,得预处理粉末;将轻烧镁粉、氮化硅铁颗粒、氮化硅铁粉、碳化硅粉混合,置于球磨机中共磨1~2h,得混合物,依次加入造纸污泥、去离子水和预处理粉末,置于混料机中混料后并困料,得基料,装入40mm×40mm的模具内,并置于压片机上,保压成型,得生坯块体,将生坯块体干燥并高温烧结处理,随炉冷却后,得硅质耐火材料。
所述的球磨超声波分散为将纳米二氧化硅粉溶于无水乙醇中,球磨1~3h,再超声波分散20~30min。
所述的混料时间为30~40min,困料时间为20~24h。
所述的保压成型为在50~80MPa下保压30~50s后成型。
所述的生坯块体的尺寸为40mm×40mm×5mm。
所述的干燥并高温烧结处理为将生坯块体置于100~120℃的烘箱中干燥8~12h后,以3℃/min的升温速率分别升温至1350℃、1400℃、1450℃、1500℃、1550℃并保温2~5h高温烧结。
本发明与其他方法相比,有益技术效果是:
(1)本发明以氮化硅铁块体作为耐火骨料,制备了硅质耐火材料,氮化硅铁是利用闪速燃烧合成技术制备的一种金属-陶瓷复合块体材料,其含有大约85%(w)的氮化硅,具有和氮化硅相似的化学稳定性与热态强度,更好的烧结性能和热导率,本发明采用无水乙醇和造纸污泥,结合超声波分散以及球磨的方式将纳米二氧化硅粉加入材料中,无水乙醇作为表面张力小的有机溶剂,可以充分洗去纳米颗粒表面的配位水分子,减少颗粒间氢键的作用,减小颗粒聚结的毛细管力,并以烷氧基取代颗粒表面的羟基团,使纳米颗粒分散更好,纳米粉分散于骨料与基质间,促进烧结,填充气孔,提高了材料的常温强度及致密性,造纸污泥中含有纤维,能显著提高材料的抗热震性;
(2)本发明中高能球磨主要是使粉末的活性增加,有利于通过机械力诱发离子固态扩散和低温出现液相,促进后期的相转变过程,由于固-固反应主要通过扩散反应,通过球磨作用,使反应物的比表面积增大,使固-固反应更容易进行;结合剂选用去离子水,轻烧镁粉遇水水化,生成氢氧化镁,起到粘结作用,且廉价而不带进任何杂质。
具体实施方式
按重量份数计,分别称取10~20份轻烧镁粉、30~50份氮化硅铁颗粒、7~12份氮化硅铁粉、5~9份碳化硅粉、1~8份纳米二氧化硅粉、20~30份去离子水、8~16份造纸污泥、10~16份无水乙醇,将纳米二氧化硅粉溶于无水乙醇中,球磨1~3h,再超声波分散20~30min后,在温度为60~80℃的烘箱中干燥至恒重,得预处理粉末;将轻烧镁粉、氮化硅铁颗粒、氮化硅铁粉、碳化硅粉混合,置于球磨机中共磨1~2h,得混合物,依次加入造纸污泥、去离子水和预处理粉末,置于混料机中混料30~40min后并困料20~24h,得基料,装入40mm×40mm的模具内,并置于压片机上,在50~80MPa下保压30~50s后成型,制备出尺寸为40mm×40mm×5mm的生坯块体,将生坯块体置于100~120℃的烘箱中干燥8~12h后,以3℃/min的升温速率分别升温至1350℃、1400℃、1450℃、1500℃、1550℃并保温2~5h高温烧结,随炉冷却后,得硅质耐火材料。
按重量份数计,分别称取10份轻烧镁粉、30份氮化硅铁颗粒、7份氮化硅铁粉、5份碳化硅粉、1份纳米二氧化硅粉、20份去离子水、8份造纸污泥、10份无水乙醇,将纳米二氧化硅粉溶于无水乙醇中,球磨1h,再超声波分散20min后,在温度为60℃的烘箱中干燥至恒重,得预处理粉末;将轻烧镁粉、氮化硅铁颗粒、氮化硅铁粉、碳化硅粉混合,置于球磨机中共磨1h,得混合物,依次加入造纸污泥、去离子水和预处理粉末,置于混料机中混料30min后并困料20h,得基料,装入40mm×40mm的模具内,并置于压片机上,在50MPa下保压30s后成型,制备出尺寸为40mm×40mm×5mm的生坯块体,将生坯块体置于100℃的烘箱中干燥8h后,以3℃/min的升温速率分别升温至1350℃、1400℃、1450℃、1500℃、1550℃并保温2h高温烧结,随炉冷却后,得硅质耐火材料。
按重量份数计,分别称取15份轻烧镁粉、40份氮化硅铁颗粒、10份氮化硅铁粉、8份碳化硅粉、5份纳米二氧化硅粉、25份去离子水、12份造纸污泥、13份无水乙醇,将纳米二氧化硅粉溶于无水乙醇中,球磨2h,再超声波分散25min后,在温度为70℃的烘箱中干燥至恒重,得预处理粉末;将轻烧镁粉、氮化硅铁颗粒、氮化硅铁粉、碳化硅粉混合,置于球磨机中共磨1h,得混合物,依次加入造纸污泥、去离子水和预处理粉末,置于混料机中混料35min后并困料22h,得基料,装入40mm×40mm的模具内,并置于压片机上,在65MPa下保压40s后成型,制备出尺寸为40mm×40mm×5mm的生坯块体,将生坯块体置于110℃的烘箱中干燥10h后,以3℃/min的升温速率分别升温至1350℃、1400℃、1450℃、1500℃、1550℃并保温3h高温烧结,随炉冷却后,得硅质耐火材料。
按重量份数计,分别称取20份轻烧镁粉、50份氮化硅铁颗粒、12份氮化硅铁粉、9份碳化硅粉、8份纳米二氧化硅粉、30份去离子水、16份造纸污泥、16份无水乙醇,将纳米二氧化硅粉溶于无水乙醇中,球磨3h,再超声波分散30min后,在温度为80℃的烘箱中干燥至恒重,得预处理粉末;将轻烧镁粉、氮化硅铁颗粒、氮化硅铁粉、碳化硅粉混合,置于球磨机中共磨2h,得混合物,依次加入造纸污泥、去离子水和预处理粉末,置于混料机中混料40min后并困料24h,得基料,装入40mm×40mm的模具内,并置于压片机上,在80MPa下保压50s后成型,制备出尺寸为40mm×40mm×5mm的生坯块体,将生坯块体置于120℃的烘箱中干燥12h后,以3℃/min的升温速率分别升温至1350℃、1400℃、1450℃、1500℃、1550℃并保温5h高温烧结,随炉冷却后,得硅质耐火材料。
对照例:东莞某公司生产的硅质耐火材料。
将实例及对照例的硅质耐火材料进行检测,具体检测如下:
显气孔率及体积密度:按照中国标准GB/T2997-2000进行。
常温耐压强度:按照GB/T5072.2-2004进行测试。
常温抗折强度试验:按照GB/T3001-2000耐火制品常温抗折强度的测试方法。
耐火度:采用GB/7322-87《耐火材料耐火度试验方法》。
具体检测结果如表1。
表1性能表征对比表
检测项目 | 实例1 | 实例2 | 实例3 | 对照例 |
显气孔率/% | 20.1 | 21.1 | 21.4 | 48.3 |
体积密度/g/cm3 | 2.51 | 2.61 | 2.73 | 1.02 |
耐压强度/MPa | 39 | 40 | 41 | 19 |
抗折强度/MPa | 16 | 17 | 18 | 8 |
耐火度/℃ | 1580 | 1585 | 1589 | 1110 |
由表1可知,本发明制备的硅质耐火材料具有良好的力学性能和物理性能。
Claims (6)
1.一种硅质耐火材料的制备方法,其特征在于具体步骤为:
按重量份数计,分别称取10~20份轻烧镁粉、30~50份氮化硅铁颗粒、7~12份氮化硅铁粉、5~9份碳化硅粉、1~8份纳米二氧化硅粉、20~30份去离子水、8~16份造纸污泥、10~16份无水乙醇,将纳米二氧化硅粉溶于无水乙醇中,球磨超声波分散后,在温度为60~80℃的烘箱中干燥至恒重,得预处理粉末;将轻烧镁粉、氮化硅铁颗粒、氮化硅铁粉、碳化硅粉混合,置于球磨机中共磨1~2h,得混合物,依次加入造纸污泥、去离子水和预处理粉末,置于混料机中混料后并困料,得基料,装入40mm×40mm的模具内,并置于压片机上,保压成型,得生坯块体,将生坯块体干燥并高温烧结处理,随炉冷却后,得硅质耐火材料。
2.根据权利要求1所述的一种硅质耐火材料的制备方法,其特征在于:所述的球磨超声波分散为将纳米二氧化硅粉溶于无水乙醇中,球磨1~3h,再超声波分散20~30min。
3.根据权利要求1所述的一种硅质耐火材料的制备方法,其特征在于:所述的混料时间为30~40min,困料时间为20~24h。
4.根据权利要求1所述的一种硅质耐火材料的制备方法,其特征在于:所述的保压成型为在50~80MPa下保压30~50s后成型。
5.根据权利要求1所述的一种硅质耐火材料的制备方法,其特征在于:所述的生坯块体的尺寸为40mm×40mm×5mm。
6.根据权利要求1所述的一种硅质耐火材料的制备方法,其特征在于:所述的干燥并高温烧结处理为将生坯块体置于100~120℃的烘箱中干燥8~12h后,以3℃/min的升温速率分别升温至1350℃、1400℃、1450℃、1500℃、1550℃并保温2~5h高温烧结。
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