CN106316448B - 一种稻壳基微孔轻质耐火材料及其制备方法 - Google Patents

一种稻壳基微孔轻质耐火材料及其制备方法 Download PDF

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CN106316448B
CN106316448B CN201610617234.XA CN201610617234A CN106316448B CN 106316448 B CN106316448 B CN 106316448B CN 201610617234 A CN201610617234 A CN 201610617234A CN 106316448 B CN106316448 B CN 106316448B
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李文凤
郭会师
韩平
叶方保
侯永改
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Henan University of Technology
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Abstract

本发明公开了一种稻壳基微孔轻质耐火材料及其制备方法。该耐火材料由稻壳、混合料和液态结合剂制成，所述混合料由以下重量百分比的原料组成：硅粉和/或硅石粉5％～40％、矿化剂3％～35％、增强剂30％～75％、增强纤维1％～15％；所述液态结合剂为亚硫酸纸浆废液和/或SiO2溶胶；所述混合料的质量为稻壳质量的15％～50％。本发明的稻壳基微孔轻质耐火材料，以农业废料稻壳为主要原料，与混合料和液态结合剂混合后制成坯料，再经成型、干燥、烧成制成成品；所用原料来源广泛，价格低廉，制备工艺简单，绿色环保；所得制品具有体积密度低、气孔率高、气孔孔径小、隔热效果好、机械强度高的优点，适合推广应用。

Description

一种稻壳基微孔轻质耐火材料及其制备方法
技术领域
本发明属于轻质耐火材料领域，具体涉及一种稻壳基微孔轻质耐火材料及其制备方法。
背景技术
轻质硅砖具有体积密度小、隔热效果好、荷重软化温度高、抗酸性气氛及抗渣侵蚀能力强等优点，作为节能保温材料被广泛应用于焦炉、热风炉、玻璃池窑等高温工业窑炉的保温层或内衬，起减少散热损失、提高窑炉工作效率、减轻炉体重量、简化炉体结构等作用。
目前，国内外制备轻质硅砖多采用添加造孔剂法或发泡法，前者是在配料时添加一定量的焦炭、锯木屑或聚合物轻球等可燃物，可燃物在坯体中占据一定空间，在高温下燃尽后于坯体中原来位置留下空隙而制得轻质硅砖；发泡法则是将发泡剂或发泡后的发泡剂添加到硅石粉料浆中搅拌制备出泡沫陶瓷料浆，再经注模、脱模、干燥和烧成制得轻质硅砖。添加造孔剂法虽简便易行，但造孔剂在试样中分布的均匀性无法有效调控，当其添加量过多时，易引起制品开裂。同时，若焦炭、锯木屑等可燃造孔剂未充分燃烧，将在制品中产生“黑心”现象，影响产品性能。发泡法虽可克服添加造孔剂法的上述缺点，但其对原料和制备工艺过程要求较为苛刻，且生产成本较高，工艺过程难以控制。
此外，传统轻质硅砖的制备均以硅石为主要原料，但硅石的主要成分为SiO2，工人长期在SiO2粉尘浓度较高的环境中作业，其身体健康受到严重威胁，极易患上近乎无法治愈的职业性肺疾病—矽肺病，不仅给病人及其家人带来痛苦，亦为国家和企业带来沉重的医疗负担。有资料显示，近年来，在一些硅砖生产性企业中，工人矽肺病的爆发率呈逐年攀升趋势。因此寻找安全环保、简便易行的高性能轻质硅砖的有效制备方法，已成为亟待解决的关键性课题。
发明内容
本发明的目的是提供一种稻壳基微孔轻质耐火材料，从而解决现有轻质硅砖制备方法存在的工艺复杂、环保性差的问题。
本发明的第二个目的是提供一种上述稻壳基微孔轻质耐火材料的制备方法。
为实现上述目的，本发明所采用的技术方案是：
一种稻壳基微孔轻质耐火材料，由稻壳、混合料和液态结合剂制成，所述混合料由以下重量百分比的原料组成：硅粉和/或硅石粉5％～40％、矿化剂3％～35％、增强剂30％～75％、增强纤维1％～15％；所述液态结合剂为亚硫酸纸浆废液和/或SiO2溶胶；所述混合料的质量为稻壳质量的15％～50％。
稻壳作为一种产量丰富且可再生的农业废弃物，具有质量轻、孔隙度大、保温性能好等特点，其化学成分为：无机成分18.8％～22.3％，挥发分60％～63％，固定碳17％～19％，水分5％～8％。无机成分主要为SiO2，来自于土壤中的硅酸或硅酸盐等可溶物，其从水稻根部进入植株后通过蒸腾流作用运输至各个部位。研究发现，土壤中的SiO2经植物再“加工”后具有结构精致、造型各异的显微结构，这种结构构筑了大量的微纳米孔隙，当稻壳在高温下充分燃尽后，SiO2粒子得以保存，并将原来的多孔网状结构保留下来，为轻质硅砖的制备提供了原料来源及天然的微纳米孔结构。且从稻壳中获取的SiO2较其它途径更经济、简捷，并可变废为宝，拓展了稻壳的综合利用。此外，稻壳中的SiO2常以无定形态存在，不会引起矽肺病的产生，绿色环保，以稻壳为主要原料制备微孔轻质硅砖是个理想的选择。
将稻壳与水混合洗净，再经干燥、破碎，即得稻壳粉。优选的，稻壳粉的粒径≤75μm。所述稻壳中SiO2的质量百分含量≥19.5％。
将硅粉和/或硅石粉、矿化剂、增强剂、增强纤维混合均匀，即得混合料。
所述增强剂为糊精粉、木质素磺酸钙、阿拉伯树胶、黄原胶、琼脂、羧甲基纤维素、SiO2凝胶粉中的一种或组合；所述增强剂的粒径均≤83μm。
所述增强纤维为聚丙烯纤维、聚丙烯腈纤维、聚乙烯纤维、聚乙烯醇纤维、聚酰胺纤维、SiO2纤维中的一种或组合；所述增强纤维的直径为25～75μm，长度为3～15mm。
所述矿化剂为CaO、CaCO3、CaF2、Na2CO3、MnO2、FeO、Fe2O3、FeCl3、FeCl2中的一种或组合。
所述液态结合剂的质量为稻壳质量的20％～120％。所述SiO2溶胶中SiO2的质量百分含量为25％～30％。
本发明的稻壳基微孔轻质耐火材料，稻壳、硅粉和/或硅石粉、矿化剂、增强剂、增强纤维、液态结合剂的配比合理，各组分协同作用；硅粉或硅石粉用量的选择可有效减小制品的烧成收缩，避免因稻壳分解使试样收缩过大而引起制品开裂；增强剂可增加坯体的结合强度，利于运输和装窑；增强纤维可防止坯体成型后因稻壳产生的弹性后效作用引起坯体开裂。
本发明的稻壳基微孔轻质耐火材料，是以农业废料稻壳为主要原料，再添加混合料、液态结合剂，经成型、干燥、烧结制成成品；其中，稻壳价格低廉且来源充足，使原料成本大大降低，且变废为宝，减少了稻壳焚烧造成的空气污染；同时，以稻壳为主要原料，其不但起提供SiO2源的作用，还发挥了天然造孔剂的作用，使制品气孔率升高；在上述原料配比的基础上，通过简单工艺即可获得性能良好的微孔硅质耐火材料，所用稻壳中SiO2为无定型态，不产生矽肺病，绿色环保。
上述稻壳基微孔轻质耐火材料的制备方法，包括以下步骤：
1)将稻壳粉、混合料和液态结合剂混合均匀，制成坯料；
2)将坯料成型制成坯体，干燥，升温至1250～1480℃烧成，即得。
步骤2)中，升温的速率为2～5℃/min，烧成的时间为3～5h。
所述成型为低压压制成型，低压压力为0.5～3MPa。
所述矿化剂的平均粒径≤47μm。
稻壳粉的平均粒径≤75μm，硅粉或硅石粉的平均粒径≤75μm；所述硅石粉中SiO2的质量百分含量≥97％；所述硅粉中Si的质量百分含量≥98％。
本发明的稻壳基微孔轻质耐火材料的制备方法，将稻壳、混合料和液态结合剂混合制成坯料，再经成型、干燥、氧化气氛下的烧结制成成品；所得成品具有体积密度低、气孔率高、气孔孔径小、隔热效果好的优点。该制备方法工艺简单、成本低廉、绿色环保，具有广阔的发展空间和应用前景，适合大规模推广应用。
具体实施方式
下面结合具体实施例对本发明作进一步说明。
以下实施例中：将稻壳与水按体积比1:5的比例混合清洗3次，去除表面泥沙，再经干燥、破碎、过筛使平均粒径≤75μm，即得稻壳粉；
硅石粉中SiO2的质量百分含量≥97％，所述硅粉中Si的质量百分含量≥98％。硅石粉、硅粉的平均粒径均≤75μm；
矿化剂中，CaO、CaCO3、CaF2、Na2CO3、MnO2、FeO、Fe2O3、FeCl3、FeCl2的平均粒径均≤47μm；
增强剂中，SiO2凝胶粉是将硅溶胶加热脱水而得；增强剂的平均粒径均≤83μm；
增强纤维中，聚丙烯纤维、聚丙烯腈纤维、聚乙烯纤维、聚乙烯醇纤维、聚酰胺纤维或SiO2纤维的直径为25～75μm、长度为3～15mm。
实施例1
本实施例的稻壳基微孔轻质耐火材料，由稻壳、混合料和液态结合剂制成，所述混合料由以下重量百分比的原料组成：硅石粉36％、CaCO3 19％、Fe2O3 6％、糊精粉34％、聚丙烯纤维5％；将硅石粉、CaCO3、Fe2O3、糊精粉、聚丙烯纤维在混料机中混合60min，即得混合料；
所述混合料的质量为稻壳质量的46％；所述液态结合剂为亚硫酸纸浆废液，添加量为稻壳质量的65％。
本实施例的稻壳基微孔轻质耐火材料的制备方法，采用以下步骤：
1)向搅拌机中加入稻壳，再加入混合料，搅拌20min；再加入亚硫酸纸浆废液，搅拌10min制成坯料；
2)将坯料在2MPa压力下机压成型，得到坯体；将坯体在110℃下干燥12h；然后以3℃/min的速率升温至1480℃并保温3h，即得稻壳基微孔轻质硅砖。
实施例2
本实施例的稻壳基微孔轻质耐火材料，由稻壳、混合料和液态结合剂制成，所述混合料由以下重量百分比的原料组成：硅石粉11％、硅粉17％、CaCO3 14％、FeCl2 3％、阿拉伯树胶21％、黄原胶22％、聚乙烯纤维12％；将硅石粉、硅粉、CaCO3、FeCl2、阿拉伯树胶、黄原胶、聚乙烯纤维在混料机中混合60min，即得混合料；
所述混合料的质量为稻壳质量的37％；所述液态结合剂为亚硫酸纸浆废液，添加量为稻壳质量的75％。
本实施例的稻壳基微孔轻质耐火材料的制备方法，采用以下步骤：
1)向搅拌机中加入稻壳粉，再加入混合料，搅拌20min；再加入亚硫酸纸浆废液，搅拌10min制成坯料；
2)将坯料在1MPa压力下机压成型，得到坯体；将坯体在110℃下干燥12h；然后以3℃/min的速率升温至1400℃并保温3h，即得稻壳基微孔轻质硅砖。
实施例3
本实施例的稻壳基微孔轻质耐火材料，由稻壳、混合料和液态结合剂制成，所述混合料由以下重量百分比的原料组成：硅石粉6％、硅粉24％、CaO 5％、MnO2 1％、Fe2O3 2％、阿拉伯树胶20％、黄原胶30％、聚乙烯纤维12％；将硅石粉、硅粉、CaO、Fe2O3、阿拉伯树胶、黄原胶、聚乙烯纤维在混料机中混合60min，即得混合料；
所述混合料的质量为稻壳质量的25％；所述液态结合剂为亚硫酸纸浆废液，添加量为稻壳质量的75％。
本实施例的稻壳基微孔轻质耐火材料的制备方法，采用以下步骤：
1)向搅拌机中加入稻壳粉，再加入混合料，搅拌20min；再加入亚硫酸纸浆废液，搅拌10min制成坯料；
2)将坯料在0.8MPa压力下机压成型，得到坯体；将坯体在110℃下干燥12h；然后以3℃/min的速率升温至1400℃并保温3h，即得稻壳基微孔轻质硅砖。
实施例4
本实施例的稻壳基微孔轻质耐火材料，由稻壳、混合料和液态结合剂制成，所述混合料由以下重量百分比的原料组成：硅石粉5％、硅粉10％、CaCO3 5％、Na2CO3 2％、SiO2凝胶粉19％、羧甲基纤维素11％、木质素磺酸钙35％、聚丙烯腈纤维4％、SiO2纤维9％；按配比取原料在混料机中混合60min，即得混合料；
所述混合料的质量为稻壳质量的20％；所述液态结合剂为SiO2溶胶(SiO2的质量百分含量为25％)，添加量为稻壳质量的75％。
本实施例的稻壳基微孔轻质耐火材料的制备方法，采用以下步骤：
1)向搅拌机中加入稻壳粉，再加入混合料，搅拌20min；再加入SiO2溶胶，搅拌10min制成坯料；
2)将坯料在0.5MPa压力下机压成型，得到坯体；将坯体在110℃下干燥12h；然后以3℃/min的速率升温至1380℃并保温3h，即得稻壳基微孔轻质硅砖。
实施例5
本实施例的稻壳基微孔轻质耐火材料，由稻壳、混合料和液态结合剂制成，所述混合料由以下重量百分比的原料组成：硅粉5％、CaF2 2％、CaO 3％、琼脂粉30％、羧甲基纤维素5％、SiO2凝胶粉40％、聚乙烯醇纤维10％、聚酰胺纤维5％；按配比取原料在混料机中混合60min，即得混合料；
所述混合料的质量为稻壳质量的20％；所述液态结合剂为SiO2溶胶(SiO2的质量百分含量为30％)，添加量为稻壳质量的120％。
本实施例的稻壳基微孔轻质耐火材料的制备方法，采用以下步骤：
1)向搅拌机中加入稻壳粉，再加入混合料，搅拌20min；再加入SiO2溶胶，搅拌10min制成坯料；
2)将坯料在3MPa压力下机压成型，得到坯体；将坯体在110℃下干燥12h；然后以2℃/min的速率升温至1250℃并保温5h，即得稻壳基微孔轻质硅砖。
试验例
本试验例检测各实施例的稻壳基微孔轻质硅砖的体积密度、显气孔率、平均孔径、常温耐压强度、热导率，结果如表1所示。
表1各实施例的稻壳基微孔轻质硅砖的性能检测结果
项目 实施例1 实施例2 实施例3 实施例4 实施例5
体积密度，g/cm<sup>3</sup> 0.68～0.72 0.50～0.60 0.44～0.47 0.20～0.27 0.72～0.75
显气孔率，％ 69.3～71.2 74.4～78.8 79.3～80.2 86.1～89.0 67.9～69.1
平均孔径，μm 0.08～0.24 0.45～0.72 0.81～1.27 2.28～4.57 0.05～0.12
常温耐压强度，MPa 8.0～12.2 4.4～6.7 2.7～3.2 0.8～1.2 11.8～15.0
热导率，W/(m·K) 0.12～0.13 0.11～0.12 0.08～0.10 0.03～0.04 0.12～0.15
由表1的试验结果可知，本发明的稻壳基微孔轻质耐火材料，气孔孔径微细，在0.05～4.57μm之间；制品体积密度低，为0.20～0.75g/cm3；气孔率高，为67.9％～89.0％；机械强度高，常温耐压强度为0.8～15.0MPa；隔热效果好，热导率为0.03～0.15W/(m·K)；使用温度高，可达1100～1450℃。所得轻质硅砖制品不但保留了稻壳间的空隙结构，还相对较完整的保留了稻壳中SiO2的天然网络骨架结构，使气孔平均孔径减小，气孔孔径分布呈现明显的双峰特征；该轻质硅砖制品具有体积密度低、气孔率高、气孔孔径小、隔热效果好、机械强度高的优点，适合推广应用。

Claims (8)

1.一种稻壳基微孔轻质耐火材料，其特征在于，由稻壳、混合料和液态结合剂制成，所述混合料由以下重量百分比的原料组成：硅粉和/或硅石粉5%～40%、矿化剂3%～35%、增强剂30%～75%、增强纤维1%～15%；所述液态结合剂为亚硫酸纸浆废液和/或SiO2溶胶；所述混合料的质量为稻壳质量的15%～50%；液态结合剂的质量为稻壳质量的20%～120%；所述增强剂为糊精、木质素磺酸钙、阿拉伯树胶、黄原胶、琼脂、羧甲基纤维素、SiO2凝胶粉中的一种或组合。
2.如权利要求1所述的稻壳基微孔轻质耐火材料，其特征在于，所述增强纤维为聚丙烯纤维、聚丙烯腈纤维、聚乙烯纤维、聚乙烯醇纤维、聚酰胺纤维、SiO2纤维中的一种或组合。
3.如权利要求1所述的稻壳基微孔轻质耐火材料，其特征在于，所述矿化剂为CaO、CaCO3、CaF2、Na2CO3、MnO2、FeO、Fe2O3、FeCl3、FeCl2中的一种或组合。
4.如权利要求1或2所述的稻壳基微孔轻质耐火材料，其特征在于，增强纤维的直径为25～75μm，长度为3～15mm。
5.一种如权利要求1所述的稻壳基微孔轻质耐火材料的制备方法，其特征在于，包括以下步骤：
1）将稻壳粉、混合料和液态结合剂混合均匀，制成坯料；
2）将坯料成型制成坯体，干燥，升温至1250～1480℃烧成，即得。
6.如权利要求5所述的制备方法，其特征在于，稻壳粉的平均粒径≤75μm，硅粉或硅石粉的平均粒径≤75μm。
7.如权利要求5所述的制备方法，其特征在于，步骤2）中，升温的速率为2～5℃/min。
8.如权利要求5所述的制备方法，其特征在于，步骤2）中，烧成的时间为3～5h。
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